CN104098228A - Organic amine wastewater treatment method - Google Patents
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Abstract
The invention provides an organic amine wastewater treatment method. According to the method, organic amine in wastewater can be removed mainly by performing pre-oxidation and anaerobic treatment on wastewater, allowing treated wastewater to pass an anoxic-aerobic biological reactor, then performing enhanced coagulation and advanced oxidation, and finally allowing the treated wastewater to pass an aerating biological filter. By the adoption of the method, toxic and harmful substances in wastewater can be foundationally removed, and difficulties in the follow-up treatment of the wastewater through a biochemical method can be reduced; the organic amine wastewater treatment method is efficient in operation, and is stable and safe in discharged water.
Description
Technical field
The present invention relates to organic amine amine field of waste water treatment, specifically a kind of removal organic amine treatment process.
Background technology
Organic amine product is broad-spectrum important industrial chemicals, mainly comprises the derived product of Monomethylamine, dimethylamine, Trimethylamine 99 and methylamine product: dimethyl formamide, N,N-DIMETHYLACETAMIDE etc.These products inevitably produce some byproducts and waste water in production building-up process, and part material also can enter factory effluent.Along with the development of China's economy, the demand of fine chemical material is increased gradually, the wastewater flow rate that these products produce in process of production also increases day by day.In organic amine factory effluent, most of material all contains amino, the feature of high COD (1g/L～10g/L) and high salinity (10～30g/L), these compositions can discharge ammonia nitrogen in biodegradation process, if directly enter natural water, probably can cause the eutrophication of water body, so this kind of waste water must effectively be processed before entering water body.
Organic amine waste water belongs to more unmanageable organism, and waste water N/C is higher, at present domestic waste water treatment process, generally adopt conventional biochemical processing process, but effect is limited, and effluent quality is not good.This treatment process is for organic amine chemistry stable in properties, and difficult for biological degradation, by adding a small amount of oxygenant preoxidation, improves the biodegradability of waste water, largely improves the removal effect of follow-up bioprocess technology to COD; For reaching emission standard organic amine bio-chemical effluent tradition, adopt oxygenant direct oxidation up to standard, though effective but expense is high, present method adopts enhanced coagulation-advanced oxidation-biological combination process for advanced treatment to process bio-chemical effluent, under identical treatment effect, reduce oxygenant consumption, reduced the cost of operation.
Summary of the invention
For the deficiency of order organic amine method of wastewater treatment, the present invention aims to provide a kind of effective organic amine method of wastewater treatment.The method specifically comprises the steps:
A. preoxidation
Organic amine waste water is carried out to preoxidation with Fenton or O3, decompose hazardous and noxious substances, improve the biodegradability of waste water; Waste water after preoxidation is adjusted to neutrality, enters settling tank precipitation 2-4 hour;
B anaerobism
Waste water through precipitation is carried out to anaerobic treatment, remove organism;
C. Anoxybiotic-aerobic biologic reactor
Anaerobic effluent is entered to Anoxybiotic-aerobic biologic reactor, remove COD and nitrogen in sewage;
D. enhanced coagulation
To Anoxybiotic-aerobic biologic reactor, enhanced coagulation is carried out in water outlet, removes the hydrophobic organic compound matter of bio-chemical effluent;
E. advanced oxidation
Water outlet after enhanced coagulation is carried out to advanced oxidation, produce the hydroxyl radical free radical (OH) with strong oxidation capacity, make macromole hardly degraded organic substance be oxidized to low toxicity or nontoxic small-molecule substance;
F. biological process advanced treatment
Advanced oxidation water outlet enters BAF, controls the residence time, dissolved oxygen, further removes COD, makes water outlet qualified discharge.
The enhanced coagulation step of this treatment process further comprises: regulate Anoxybiotic-aerobic biologic reactor water outlet PH to 4-8, according to the ratio of 100-400mg/L, add bodied ferric sulfate and carry out coagulation, stir 15 minutes, according to 2-4mg/L ratio, add polyacrylamide, then enter settling tank precipitation.
The advanced oxidation of this treatment process can adopt following steps:
With Fenton, regulate pH value to 1-5 the water outlet of enhanced coagulation, wherein, H2O2 dosage 100-600mg/L, and the ratio between 1/10-1/6 adds ferrous sulfate according to Fe2+/H2O2, oxidation 1-6 hour, adds alkali and regulates PH to neutral after oxidation, water outlet enters settling tank precipitation.
The advanced oxidation of this treatment process also can adopt following steps:
Anoxybiotic-aerobic biologic reactor is gone out to water ph value and be adjusted to 7-10, according to 100-400mg/L, add O3, use low pressure ultraviolet ray to irradiate simultaneously, reaction 1-4 hour.
The step C of present method also comprises, anoxic denitrification technique residence time HRT >=24 hour, aerobe reactor load 0.1-0.2kgCOD/kgMLSS.d, sludge concentration MLSS >=4000mg/L, dissolved oxygen is controlled at 2-4mg/L, hydraulic detention time HRT >=24 hour, second pond mud is back to anoxic pond by 50-80%, denitrification internal reflux ratio 200-400%.
In the step F of present method, waste water pH value in BAF is 6-8, dissolved oxygen 2-5mg/L, retention time of sewage >=6h.
Organic amine described in present method is: N methyldiethanol amine, DMF, N-N,N-DIMETHYLACETAMIDE, trolamine.
Present method can adopt USAB or ABR anaerobic treatment process, anaerobism temperature 30-40 ℃, and anaerobism volumetric loading 3-6kgCOD/m3.d, waste water PH is controlled between 7-8.
Accompanying drawing explanation
Fig. 1 present method is carried out the schematic flow sheet of organic amine wastewater treatment.
Embodiment
For making the object, technical solutions and advantages of the present invention more cheer and bright, below in conjunction with embodiment and with reference to accompanying drawing, the present invention is described in more detail.Should be appreciated that, these descriptions are exemplary, and do not really want to limit the scope of the invention.In addition, in the following description, omitted the description to known configurations and technology, to avoid unnecessarily obscuring concept of the present invention.
For overcoming problems of the prior art, organic amine waste water treatment process involved in the present invention adopts " preoxidation-anaerobic-anoxic/aerobe reactor-enhanced coagulation/advanced oxidation-biological advanced treatment " combination process, and concrete technical scheme is as follows:
1 preoxidation: can adopt two kinds of methods: 1. hydrogen peroxide (H2O2) oxidation capacity is limited separately, adopt Fenton oxidation to its essence is that H2O2 generates the hydroxyl radical free radical (OH) with high reaction activity under the katalysis of Fe2+, OH can make its degraded with most of organism effects, Fenton oxidation acid adding (hydrochloric acid, sulfuric acid) regulate PH to 1-5, H2O2 dosage 100-400mg/L, ferrous sulfate adds by Fe2+/H2O2 mol ratio 1/10-1/6, oxidization time 1-4 hour, after oxidation, add alkali (sodium hydroxide or lime) and be adjusted to neutrality, enter settling tank precipitation 2-4 hour, 2. O3 oxidation, adds acid-alkali accommodation PH to 7-10, dosage 100-600mg/L, oxidization time 1-4 hour.
2. anaerobism can adopt the anaerobic treatment process such as UASB or ABR, and waste water keeps anaerobism temperature 30-40 ℃ with steam, anaerobism volumetric loading 3-6kgCOD/m3.d, and waste water PH is controlled between 7-8, residence time HRT >=24 hour.
3. anaerobic effluent enters Anoxybiotic-aerobic biologic reactor, anoxic section is for denitrogenation, aerobic section is for removing the organism of water, ammonia nitrogen is oxidized to nitric nitrogen simultaneously, anoxic denitrification technique hydraulic detention time 24-48 hour, be controlled at≤0.5mg/L of dissolved oxygen, (implication of sludge loading aspect microbial metabolism is exactly F/M ratio to aerobe reactor load 0.1-0.2kgCOD/kgMLSS.d, the amount of the pollutent that the active sludge of representation unit quality is removed within the unit time, units/kg COD (BOD)/kg mud d), sludge concentration MLSS >=8000mg/L, dissolved oxygen is controlled at 2-4mg/L, PH is controlled between 7-8, hydraulic detention time HRT >=24 hour, second pond mud is back to anoxic pond by 50-80%, denitrification internal reflux ratio 200-400%, if with membrane bioreactor membrane flux 10-20L/m2.h, denitrification internal reflux ratio 200-400%.
4. enhanced coagulation
Enhanced coagulation is point in source water dosing coagulant and control certain pH value, thereby organic removal effect in raising conventional processing, the water outlet of Anoxybiotic-aerobic biologic reactor is added to acid-alkali accommodation PH to 4-8, add 100-400mg/L bodied ferric sulfate (PFS) coagulation, churning time 15 minutes, add 2-4mg/L anionic polyacrylamide (PAM) and contribute to flco to become large, after enter settling tank residence time 2-4 hour.
5. advanced oxidation
Coagulation water outlet can adopt two kinds of methods to carry out advanced oxidation, 1. Fenton oxidation: coagulation water outlet acid adding regulates PH to 1-5, H2O2 dosage 100-600mg/L, ferrous sulfate adds by Fe2+/H2O2 mol ratio 1/10-1/6, oxidization time 1-6 hour, water outlet adds alkali and regulates PH to 7-9, enters settling tank precipitation 2-4 hour; 2. a lot of petroleum chemical enterprises consider to forbid transportation and storage oxygenant (H2O2 from security standpoint, clorox), therefore can adopt online generation oxygenant technology ultraviolet-ozone oxidation, with acid and alkali, regulate PH to 7-10, low pressure ultraviolet lamp 15-45KW, ultraviolet wavelength 254nm, ultra violet lamp passes into O3 simultaneously, O3 dosage 100-400mg/L, reaction times 1-4 hour, O3 produces OH under the effect of ultraviolet, the hydrophilic organics hydrophilicity of difficult degradation in oxidized waste water, and the biodegradability of waste water improves simultaneously.
6. BAF is a kind of aerobic activated sludge and the technology of filtering combination, there is working cost low, effluent quality is the feature such as safely, waste water pH value in BAF is 6-8, adopt 2-4mm haydite to do filler, the residence time is greater than 6 hours, and dissolved oxygen is controlled at 2-5mg/L, once, water outlet reaches outer row's standard in back flushing in 24-72 hour.
Embodiment 1
At present, the de-H2S of oil refinery dry gas adopts alcohol amine absorption process more, and hydramine is mainly thanomin, diethanolamine, trolamine and N methyldiethanol amine, wherein uses comparatively generally N methyldiethanol amine.Compare with traditional method, alcohol amine absorption process has the advantages such as desulfuration efficiency is high, technical process simple, absorption liquid loop cycle is long.Because absorption liquid recycles, in device steady running process, can not produce the waste water containing hydramine, but device shutting down or be affected by other factors and while causing the fluctuation of certain operations, can cause the discharge of part hydramine, the Wastewater Treated by Activated Sludge Process process to downstream when sewage work impacts.
N methyldiethanol amine waste liquid COD7000-10000mg/L, TN=400-450mg/L, TDS=1%-3%, adopts present method anaerobic UASB-anoxic/aerobic membrane bioreactor-enhanced coagulation-UV/ozone oxidation-BAF; UASB temperature 30-35 ℃, residence time HRT=48 hour, volumetric loading 6kgCOD/m3.d; Waste water is in the residence time of anoxic section HRT=24 hour, dissolved oxygen≤0.5mg/L, internal reflux ratio 300%; Membrane bioreactor hydraulic detention time HRT=48 hour, sludge concentration 10400mg/L, sludge loading 0.17kgCOD/kgMLSS.d, dissolved oxygen 3-4mg/L, flat sheet membrane membrane flux 15L/m2.h; Bodied ferric sulfate coagulation PH is 5, and dosage 250mg/L, precipitates 2 hours at 15 minutes coagulation time; Ultraviolet-ozone reaction PH=10,, low pressure ultraviolet lamp 15KW, ultraviolet 254nm, the reacting weight 300mg/L of O3,2 hours reaction times; BAF dissolved oxygen is 3-4mg/L, residence time HRT=8 hour.Get the water outlet of each processing unit and carry out COD, NH3-N detection, test-results is as table 1.
Table 1 is used processing unit provided by the invention in the removal process of each unit COD and TN, NH3-N
Embodiment 2
DMF (N, N-dimethylformamide are called for short DMF) is a kind of organic solvent of excellent property, can dissolve each other with water and most organic solvent, therefore has the title of menstruum universale, in chemical industry, has a wide range of applications.China's Occupational Exposure harm of poison grading determines that DMF is II level (moderate harm), and the U.S. determines that DMF is that human body may carcinogenic substance.DMF waste water enters in water and can cause biological chemistry oxygen-consumption and nitrogen content to increase, and water quality is worsened rapidly, and be difficult to biological degradation, the at present domestic and international rarely seen report to DMF purification of waste water and processing.Therefore it is very necessary the waste water that contains DMF being processed
N methyldiethanol amine waste water COD 7000-10000mg/L, TN=400-450mg/L, adopts O3 preoxidation-anaerobic UASB-anoxic/aerobic membrane bioreactor-enhanced coagulation-Fenton oxidizing-biological biological filtering tank.O3 preoxidation dosage 300mg/L,, reaction PH=10,2 hours reaction times; UASB temperature 30-35 ℃, residence time HRT=48 hour, volumetric loading 3-5kgCOD/m3.d; Waste water is in the residence time of anoxic section HRT=24 hour, dissolved oxygen≤0.5mg/L, internal reflux ratio 300%; Membrane bioreactor hydraulic detention time HRT=48 hour, sludge concentration 9200mg/L, sludge loading 0.18 kgCOD/kgMLSS.d, dissolved oxygen 3-4mg/L, flat sheet membrane membrane flux 15L/m2.h; Enhanced coagulation bodied ferric sulfate coagulation PH is 5, dosage 250mg/L; Fenton oxidation regulates PH=3.5, H2O2 dosage 200-400mg/L, and ferrous sulfate adds by Fe2+/H2O2 mol ratio 1/6, oxidization time 2 hours, water outlet regulates PH to neutral, enters settling tank precipitation HRT=4 hour; BAF dissolved oxygen=3mg/L, residence time HRT=12 hour.Get the water outlet of each processing unit and carry out COD, NH3-N detection, test-results is as table 2.
Table 2 is used processing unit provided by the invention in the removal process of each unit COD and NH3-N
Embodiment 3
A methylamine waste liquid, waste water COD 5000-6000mg/L, TN=200-360mg/L; Adopt anaerobic UASB-anoxia/aerobic biological reactor-enhanced coagulation-Fenton oxidizing-biological biological filtering tank.UASB temperature 30-35 ℃, residence time HRT=24 hour, volumetric loading 5-6kgCOD/m3.d; Waste water is in the residence time of anoxic section HRT=24 hour, dissolved oxygen≤0.5mg/L, return sludge ratio 60%, internal reflux ratio 300%; Aerobe reactor hydraulic detention time HRT=48 hour, sludge concentration 5000mg/L, sludge loading 0.15kgCOD/kgMLSS.d, dissolved oxygen 3-4mg/L; Enhanced coagulation bodied ferric sulfate coagulation PH is 7, dosage 250mg/L, and Fenton oxidation regulates PH=3.5, H2O2=200-400mg/L, ferrous sulfate adds by Fe2+/H2O2 mol ratio 1/6, oxidization time 2 hours, water outlet regulates PH to neutral, enters settling tank precipitation HRT=4 hour; BAF dissolved oxygen=3mg/L, residence time HRT=8 hour.Get the water outlet of each processing unit and carry out COD, NH3-N detection, test-results is as table 3.
Table 3 is used processing unit provided by the invention in the removal process of each unit COD and NH3-N
Claims (8)
1. a treatment process for organic amine waste water, is characterized in that treatment step is as follows:
A. preoxidation
Organic amine waste water is carried out to preoxidation with Fenton or O3, decompose hazardous and noxious substances, improve the biodegradability of waste water; Waste water after preoxidation is adjusted to neutrality, enters settling tank precipitation 2-4 hour;
B anaerobism
Waste water through precipitation is carried out to anaerobic treatment, remove organism;
C. Anoxybiotic-aerobic biologic reactor
Anaerobic effluent is entered to Anoxybiotic-aerobic biologic reactor, remove COD and nitrogen in sewage;
D. enhanced coagulation
To Anoxybiotic-aerobic biologic reactor, enhanced coagulation is carried out in water outlet, removes the hydrophobic organic compound matter of bio-chemical effluent;
E. advanced oxidation
Water outlet after enhanced coagulation is carried out to advanced oxidation, produce the hydroxyl radical free radical (OH) with strong oxidation capacity, make macromole hardly degraded organic substance be oxidized to low toxicity or nontoxic small-molecule substance;
F. biological process advanced treatment
Advanced oxidation water outlet enters BAF, controls the residence time, dissolved oxygen, further removes COD, makes water outlet qualified discharge.
2. treatment process according to claim 1, is characterized in that described enhanced coagulation step comprises:
Regulate Anoxybiotic-aerobic biologic reactor water outlet PH to 4-8, according to the ratio of 100-400mg/L, add bodied ferric sulfate and carry out coagulation, stir 15 minutes, according to 2-4mg/L ratio, add polyacrylamide, then enter settling tank precipitation.
3. treatment process according to claim 2, is characterized in that described advanced oxidation step comprises:
With Fenton, regulate pH value to 1-5 the water outlet of enhanced coagulation, wherein, H2O2 dosage 100-600mg/L, and the ratio between 1/10-1/6 adds ferrous sulfate according to Fe2+/H2O2, oxidation 1-6 hour, adds alkali and regulates PH to neutral after oxidation, water outlet enters settling tank precipitation.
4. treatment process according to claim 2, is characterized in that described advanced oxidation comprises:
Anoxybiotic-aerobic biologic reactor is gone out to water ph value and be adjusted to 7-10, according to 100-400mg/L, add O3, use low pressure ultraviolet ray to irradiate simultaneously, reaction 1-4 hour.
5. according to the treatment process described in claim 3 or 4, it is characterized in that described step C also comprises, anoxic denitrification technique residence time HRT >=24 hour, aerobe reactor load 0.1-0.2kgCOD/kgMLSS.d, sludge concentration MLSS >=4000mg/L, dissolved oxygen is controlled at 2-4mg/L, hydraulic detention time HRT >=24 hour, second pond mud is back to anoxic pond by 50-80%, denitrification internal reflux ratio 200-400%.
6. treatment process according to claim 4, is characterized in that in described treatment step F, waste water pH value in BAF is 6-8, dissolved oxygen 2-5mg/L, retention time of sewage >=6h.
7. treatment process according to claim 4, is characterized in that described organic amine is: N methyldiethanol amine, DMF, N-N,N-DIMETHYLACETAMIDE, trolamine.
8. treatment process according to claim 4, is characterized in that in described treatment step B: can adopt USAB or ABR anaerobic treatment process, and anaerobism temperature 30-40 ℃, anaerobism volumetric loading 3-6kgCOD/m3.d, waste water PH is controlled between 7-8.
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