CN102161537A - Deep purification method of coking wastewater based on advanced ozone oxidation - Google Patents
Deep purification method of coking wastewater based on advanced ozone oxidation Download PDFInfo
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- CN102161537A CN102161537A CN 201010237749 CN201010237749A CN102161537A CN 102161537 A CN102161537 A CN 102161537A CN 201010237749 CN201010237749 CN 201010237749 CN 201010237749 A CN201010237749 A CN 201010237749A CN 102161537 A CN102161537 A CN 102161537A
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Abstract
The invention discloses a deep purification method of coking wastewater based on advanced ozone oxidation, belonging to the field of wastewater treatment, and particularly relating to a deep purification method for the effluent of the biochemical treatment facilities of coking plants. Aiming at the problem in the prior art, the invention provides a method for coupling homogeneous catalysis and non-homogeneous catalysis for ozone so as to realize deep purification of the effluent of the biochemical treatment facilities of coking wastewater. In the deep purification method, wastewater of which the pH value is 8-12 is subjected to homogeneous catalysis reaction in the presence of ozone and hydrogen peroxide; non-homogeneous catalysis is carried out in the presence of the non-homogeneous catalyst; thus, processed effluent COD (Chemical Oxygen Demand) is less than 100mg/L; and thus the processed effluent does not cause secondary pollution to environment.
Description
Technical field
The present invention relates to the treatment process of coking chemical waste water, the deep treatment method of particularly a kind of coke-oven plant's biochemical treatment facility water outlet belongs to field of waste water treatment.
Background technology
China is coke production and consumption big country, especially obtains fast development in coke production capacity in recent years.Coke output was 33,554 ten thousand tons in 2007, accounted for 60% of global coke ultimate production.Coking chemical waste water is that the coal Pintsch process obtains coke and coal gas and reclaim in process of production in the byproduct processes such as prepared tar, benzene producing.Because of being subjected to raw coal character, coking temperature, coke chemicals to reclaim influence of various factors such as technology, the coking chemical waste water complicated component, contain and multiplely be difficult to be degraded by microorganisms or inorganic salts such as the organism of bio-toxicity and a large amount of ammonium salt, sulfide, prussiate are arranged, be one of important source of pollution that cause water pollution, be a more scabrous problem in Industrial Wastewater Treatment always.
Its main source has: 1. remained ammonia.Form by the compound that produces in the moisture of coking and the process of coking.Under the normal circumstances, its quantity accounts for the over half of whole waste water.2. Chemicals process drain.Comprise Chemicals reclaim with treating process in the branch regular draining of dried up and various storage tanks and the accident draining of each relevant workshop section.3. the whole cold water of crude benzol and coal gas desulfurization and gas final cold round-robin sewer.Phenol, cyanogen, benzene, sulfide and the pyridinium salt etc. that wherein contain some amount.
Coking chemical waste water contains a large amount of hazardous and noxious substances, as not treated or not exclusively just discharging of processing, will cause great harm to environment.As prussiate is highly toxic substance, enters organism and can cause poisoning; Many carcinogenic mutagenic matters that are listed in are arranged in polycyclic aromatic hydrocarbons and the heterogeneous ring compound; Some phenolic compound can cause the cell protein sex change, and high ammonia nitrogen can cause serious body eutrophication, and denitrogenation not exclusively and the NO that generates
2-It also is carcinogenic mutagenic matter; Large amount of organic enters water body meeting serious harm hydrobiont etc.Therefore, administer coking chemical waste water, realize that qualified discharge has profound significance.
The treatment process of coking chemical waste water can be divided into three grades according to concentration of narmful substance (mainly being the concentration of phenol): process for primary treatment mainly contains solvent extration dephenolize and the dephenolize of steam cycle method, mainly handles high-concentration phenolic wastewater; The second-stage treatment method mainly is a biochemical treatment process, also is activated sludge process, mainly handles the phenolic wastewater of intermediate concentration; The tertiary treatment method mainly contains active carbon adsorption and ozone oxidation method.Tertiary treated wastewater derives from the water after the second-stage treatment, is along with environmental requirement improves and the water processing establishment that is provided with day by day.
At present, domestic and international processing to coking chemical waste water mainly is based on biological process.Biological treatment has advantages such as the water yield of processing is big, working cost is low, the removal pollution range is wide, and is better to the treatment effect of pollutents such as phenol, cyanogen.But, along with the raising of people's environmental consciousness, formulated more strict pollutant emission standard, the coking chemical waste water after the traditional biological facture is handled has been difficult to reach emission standard.Since the nineties, various countries all improve to some extent on the treatment technology to coking chemical waste water, all in the possibility of inquiring into Zero-discharge coked wastewater.Therefore, seeking technology three grades of advanced treatment technology simple, with low cost is problems that present Treatment of Coking Effluent presses for solution.But the tertiary treatment of waste water has investment greatly, the characteristics that process cost is high.
After traditional bioprocess technology is handled, still contain the organism of higher concentration in the water outlet.The material that the amounts of residual contamination do great majority are biological strong toxicity, environmental hazard is big, as furans, piperidines, pyridine, narrow more than 50 kind of Polycyclic aromatic hydrocarbons such as azoles, carbazole, thiophene, polychlorobiphenyl, quinoline, naphthylamines, phenol and heterocycle organism, some in addition be persistence organic pollutant (POPs), wastewater biodegradability after the biological treatment and enzyme property while still alive are all poor, be difficult to biological degradation, still water body polluted.The ozone oxidation method can further be removed organism as a kind of effective advanced treatment technology, satisfies the water outlet emission standard of increasingly stringent.
Ozone is a kind of strong oxidizer, can react rapidly with most of organism, microorganism in the waste water, can remove pollutents such as phenol in the waste water, cyanogen, and reduces COD, BOD value, also can play decolouring, deodorizing, germ-resistant effect simultaneously.The strong oxidizing property of ozone can be removed pollutants in waste water quickly and efficiently, and ozone is decomposed into oxygen very soon in water, can not cause secondary pollution, and operational administrative is simple and convenient.Because also there is the shortcoming that investment is high, power consumption is big, processing cost is high in this method, the ozone oxidation method also is mainly used in the advanced treatment of waste water at present.
Chinese invention patent 200910042993.8 discloses the method that a kind of in-depth coking wastewater and biochemical tail water is handled, it be with the coking chemical waste water biochemical tail water after equalizing tank is regulated PH with alkaline matter and is 9～12, add high-efficient oxidant (ozone etc.) and carry out oxide treatment, mixed solution carries out adsorption treatment through after the precipitate and separate again to filtrate.This method need filter and handle through separating for several times, and this method do not provide the consumption of material such as oxygenant, simultaneously in implementation process, and OH
-As just the pH regulator agent, do not utilize its catalysed oxidn for oxygenant, cause the oxygenant dosage excessive, and the utilising efficiency of oxygenant is low, cost is higher.
China utility model cn200720051783.1 discloses a kind of ozone heterogeneous catalytic oxidation water treatment device, and its heterogeneous catalytic oxidation filler is by γ-Al
2O
3Load Fe
2O
3Form, but the utility model is only with regard to Al
2O
3The General Principle of carrying transition metal is set forth, and does not propose concrete composition and consumption; And, at O
3Catalytic oxidation process in, simple heterogeneous catalysis can not reach high processing efficient.
Summary of the invention
The objective of the invention is at waste water after the biochemical treatment not up to standard, and existing processing step complexity, the unfavorable problem of oxidation effectiveness, the homogeneous catalysis and the heterogeneous catalysis coupling process of ozone have been proposed, realize the deep purifying of coking chemical waste water biochemical reaction facility water outlet, and cost is low, effective, continuously Treatment of Wastewater in Coking.
The object of the invention is achieved through the following technical solutions:
(a) regulating waste water ph in equalizing tank 1 is 8～12;
(b) add ozone and hydrogen peroxide in the waste water behind the adjust pH, every liter of waste water adds 140～400mg O
3, H
2O
2With O
3The mol ratio of add-on is 0.5～1.4;
(c) waste water that adds ozone and hydrogen peroxide carries out oxide treatment in oxidation reactor 6, filling solid heterogeneous catalyst in the oxidation reactor 6, the solid heterogeneous catalyst volume is 1: 3～1: 6 with the ratio of oxidation reactor 6 volumes, and the hydraulic detention time of waste water in oxidation reactor is 5～20 minutes;
(d) the directly discharging after filtration of the waste water after the processing.
In the present invention, oxide treatment to waste water mainly is to utilize the advanced oxidation function of ozone, the adding mode of ozone is removed aeration mode commonly used and is added the waste water China and foreign countries, can also between equalizing tank 1 and oxidation reactor 6, increase a mixing jet device 5, be connected with ozonizer 4 and dioxygen tank 3 on the mixing jet device 5, ozonizer 4 can produce ozone, when waste water when equalizing tank 1 is flowed through mixing jet device 5, open ozonizer 4, ozone concn in the ozonizer 4 exit end gases is controlled to be 70～100mg/L, and the gas of ozonizer 4 exit end promptly enters the gas of mixing jet device 5; Open dioxygen tank 3 simultaneously, in the waste water of mixing jet device 5, drip the catalyzer of hydrogen peroxide as ozone oxidation; When waste water is flowed through mixing jet device 5, can produce negative pressure, utilize this negative pressure gas ozoniferous and hydrogen peroxide can be sucked in the mixing jet device 5; The gas flow ozoniferous that mixing jet device 5 sucks is 2: 1～4: 1 with the ratio by the wastewater flow in the mixing jet device; Waste water enters oxidation reactor 6 in mixing jet device 5 with after ozone, hydrogen peroxide mix.
In the present invention,, increase the gas-liquid two-phase contact area simultaneously, promote the rate of mass transfer of ozone molecule, so the solid heterogeneous catalyzer of filling is selected Al for use in the oxidation reactor 6 to liquid phase because metallic element can improve the generating rate of hydroxyl radical free radical OH effectively
2O
3Load Fe
2O
3, in addition, can also select TiO for use
2Load MnO
xCatalyzer Deng transition metal.
Hydrogen peroxide is best in the mode that at the uniform velocity drips.
Ozone, hydrogen peroxide, waste water generally also have small amount of ozone and overflow after fully reacting in oxidation reactor 6, can discharge through behind the heating pyrolyze; Perhaps adopt way of recycling to utilize again, specifically be after ozone, hydrogen peroxide, waste water fully react in oxidation reactor 6, enter two phase separator 9, by water pump 10 waste water in the two phase separator 9 is pumped into mixing jet device 11, when waste water is flowed through mixing jet device 11, can produce negative pressure, can utilize this negative pressure that the ozone of overflowing in the two phase separator 9 is sucked, and in mixing jet device 11, enter oxidation reactor 6 after the dissolving once more, react once more with waste water, hydrogen peroxide in the oxidation reactor 6, realize utilization once more ozone.
According to the decomposition mechanism of ozone, under alkaline condition, ozone oxidation is through radical mechanism, OH
-Can decompose generation secondary oxidation agent hydroxyl radical free radical OH by catalysis ozone, OH has the oxidation capacity stronger than ozone, the fast and non-selectivity of speed of response.Under alkaline condition, the acid product that alkali has neutralized and generated in the reaction process has reduced the generation of free radical inhibitors in addition, has promoted the forward of reaction to carry out, and helps the raising of COD clearance.Therefore, with strong oxidizer H
2O
2Introduce O
3Reaction system is compared H with single oxidising process
2O
2Accelerate the formation of OH, can significantly improve degradation speed.
Among the present invention, handle back water outlet COD＜100mg/L, chroma removal rate, sulfide clearance are near 100%, to the environment non-secondary pollution.
Description of drawings
Fig. 1 is the schematic flow sheet of the coking waste water treatment method of the direct cracking discharging of ozone.
Fig. 2 is the schematic flow sheet of the coking waste water treatment method of ozone recycling.
1-equalizing tank 2-sump pump 3-dioxygen tank 4-ozonizer
5-mixing jet device 6-oxidation reactor 7-strainer 8-water outlet
9-two phase separator 10-water pump 11-mixing jet device 12-offgas duct
The 13-cracker
Embodiment
Embodiment one
To send into equalizing tank 1 through the coking chemical waste water of biochemical treatment, flow 1m
3/ h, regulating waste water ph with unslaked lime in equalizing tank 1 is 8, opens water pump 2, and waste water is pumped into oxidation reactor 6, adds gas ozoniferous at oxidation reactor 6, flow is 2m
3/ h, O in the gas
3Concentration is 70mg/L, and promptly every liter of waste water adds ozone 140mg; Add concentration simultaneously and be 30% hydrogen peroxide, H
2O
2With O
3The mol ratio of add-on is 0.5; 53L Al is housed in the oxidation reactor 6
2O
3Load Fe
2O
3The solid heterogeneous catalyzer, oxidation reactor 6 volumes are 1: 3 with solid heterogeneous catalyst volume ratio, hydraulic detention time is 5 minutes.
Waste water after the oxide treatment is filtered the back discharging through filter 7, and water outlet COD effluxes after reaching national grade one discharge standard.The tail gas that contains drop ozone discharges after through 10 cracking of heating pyrolyze device.
Embodiment two
To send into equalizing tank 1 through the coking chemical waste water of biochemical treatment, flow is 5L/min, regulating waste water ph with NaOH in equalizing tank is 12, open water pump 2, waste water is pumped into mixing jet device 5 from equalizing tank 1, open ozonizer 4 simultaneously, the adjustments of gas flow is 20L/min, make that the ratio of the wastewater flow in gas flow and the mixing jet device 5 of flowing through of foul smell producer 4 exit end is 4: 1, ozone concn is 100mg/L in the gas; Open dioxygen tank 3 simultaneously, adding concentration is 27% hydrogen peroxide, H
2O
2With O
3The mol ratio of add-on is 1.4.Waste water, ozone, hydrogen peroxide enter in the oxidation reactor 6, and hydraulic detention time is 20 minutes, and 27L TiO is housed in the oxidation reactor 6
2Load MnO
xThe solid heterogeneous catalyzer, oxidation reactor 6 volumes are 1: 6 with solid heterogeneous catalyst volume ratio.
Waste water after the oxide treatment is filtered the back discharging through filter 7.The tail gas that contains drop ozone discharges after through 10 cracking of heating pyrolyze device.
Embodiment three
To send into equalizing tank 1 through the coking chemical waste water of biochemical treatment, flow 10L/min, regulating waste water ph with NaOH in equalizing tank is 10, open water pump 2, waste water is pumped into mixing jet device 5 from equalizing tank 1, open ozonizer 4 simultaneously, the adjustments of gas flow is 30L/min, make that the ratio of the wastewater flow in gas flow and the mixing jet device 5 of flowing through of foul smell producer 4 exit end is 3: 1, ozone concn is 80mg/L in the gas; Open dioxygen tank 3 simultaneously, adding concentration is 27% hydrogen peroxide, H
2O
2With O
3The mol ratio of add-on is 1.Waste water, ozone, hydrogen peroxide enter in the oxidation reactor 6, and hydraulic detention time is 10 minutes, and 40L Al is housed in the oxidation reactor 6
2O
3Load Fe
2O
3The solid heterogeneous catalyzer, oxidation reactor 6 volumes are 1: 4 with solid heterogeneous catalyst volume ratio.
After ozone, hydrogen peroxide, waste water fully react in oxidation reactor 6, put into two phase separator 9, by water pump 10 waste water in the two phase separator 9 is pumped into mixing jet device 11, when waste water is flowed through mixing jet device 11, can produce negative pressure, can utilize this negative pressure that the ozone of overflowing in the two phase separator 9 is sucked, and in mixing jet device 11, enter oxidation reactor 6 after the dissolving once more, realize utilization once more ozone.Remaining waste water inflow filter 7 in the two phase separator 9, discharging after filtering.
Embodiment four
To send into equalizing tank 1 through the coking chemical waste water of biochemical treatment, flow is 5L/min, regulating waste water ph with NaOH in equalizing tank is 9, open water pump 2, waste water is pumped into mixing jet device 5 from equalizing tank 1, open ozonizer 4 simultaneously, the adjustments of gas flow is 10L/min, make that the ratio of the wastewater flow in gas flow and the mixing jet device 5 of flowing through of foul smell producer 4 exit end is 2: 1, ozone concn is 80mg/L in the gas; Open dioxygen tank 3 simultaneously, adding concentration is 27% hydrogen peroxide, H
2O
2With O
3The mol ratio of add-on is 1.2.Waste water, ozone, hydrogen peroxide enter in the oxidation reactor 6, and hydraulic detention time is 20 minutes, and 27L TiO is housed in the oxidation reactor 6
2Load MnO
xThe solid heterogeneous catalyzer, oxidation reactor 6 volumes are 1: 6 with solid heterogeneous catalyst volume ratio.
Waste water after the oxide treatment is filtered the back discharging through filter 7.The tail gas that contains drop ozone discharges after through 10 cracking of heating pyrolyze device.
Claims (6)
1. the coking wastewater deep purifying method based on ozone high grade oxidation is characterized in that, comprises the steps:
(a) regulating waste water ph is 8～12;
(b) add ozone and hydrogen peroxide in the waste water behind the adjust pH, every liter of waste water adds 140～400mg O
3, H
2O
2With O
3The mol ratio of add-on is 0.5～1.4;
(c) waste water that adds ozone and hydrogen peroxide carries out oxide treatment in oxidation reactor (6), the interior filling solid heterogeneous catalyst of oxidation reactor (6), the ratio of solid heterogeneous catalyst volume and oxidation reactor (6) volume is 1: 3～1: 6, and the hydraulic detention time of waste water in oxidation reactor is 5～20 minutes;
(d) the directly discharging after filtration of the waste water after the processing.
2. a kind of coking wastewater deep purifying method according to claim 1 based on ozone high grade oxidation, it is characterized in that, the adding mode of ozone and hydrogen peroxide is in the described step (b): the waste water behind the adjust pH pumps into mixing jet device (5), is connected with ozonizer (4) and dioxygen tank (3) on the mixing jet device (5); When waste water is flowed through mixing jet device (5), open ozonizer (4), ozone concn in ozonizer (4) the exit end gas is controlled to be 70～100mg/L, and the gas flow of mixing jet device (5) suction is 2: 1～4: 1 with the ratio by the wastewater flow in the mixing jet device (5); Open dioxygen tank (3) simultaneously, in the waste water of mixing jet device (5), drip hydrogen peroxide; Waste water enters oxidation reactor (6) in mixing jet device (5) with after ozone, hydrogen peroxide mix.
3. a kind of coking wastewater deep purifying method based on ozone high grade oxidation according to claim 1 and 2 is characterized in that described solid heterogeneous catalyzer is Al
2O
3Load Fe
2O
3Solid material.
4. a kind of coking wastewater deep purifying method based on ozone high grade oxidation according to claim 1 and 2 is characterized in that, at the uniform velocity drips hydrogen peroxide.
5. a kind of coking wastewater deep purifying method based on ozone high grade oxidation according to claim 1 and 2 is characterized in that the drop ozone recycling in the oxidation reactor (6).
6. a kind of coking wastewater deep purifying method according to claim 5 based on ozone high grade oxidation, it is characterized in that, described recycling step is: after ozone, hydrogen peroxide, waste water fully react in oxidation reactor (6), enter two phase separator (9), by water pump (10) waste water in the two phase separator (9) is pumped into mixing jet device (11), utilize negative pressure that the ozone of overflowing in the two phase separator (9) is sucked, and in mixing jet device (11), enter oxidation reactor (6) after the dissolving once more.
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Application publication date: 20110824 |