CN101985379A - Treatment method for high-concentration sulfur-containing caustic sludge wastewater from oil refinery - Google Patents
Treatment method for high-concentration sulfur-containing caustic sludge wastewater from oil refinery Download PDFInfo
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Abstract
The invention relates to a treatment method for high-concentration sulfur-containing caustic sludge wastewater from an oil refinery. The main process comprises precipitation, acidification, electrocoagulation and Fenton reagent oxidation. The method comprises the following steps of: adding a precipitator into the high-concentration sulfur-containing caustic sludge wastewater refined from the oil refinery so as to remove sulfide, sulfur ether, sulfur alcohol and other malodorants, greatly reduce odor of caustic residue and reduce toxicity of water body; then acidifying and recovering crude phenol and naphthenic acid; and performing oxidation treatment through an electrocoagulation-Fenton reagent so as to remove most of the polluted and nonbiodegradable organic matters from the wastewater. The limit of COD concentration and sulfur content of water inlet is improved to the greatest degree, the need of a large amount of dilution water is saved in the conventional operation process, the crude phenol and naphthenic acid in the caustic residue wastewater are effectively recovered, and no secondary pollution is produced in the operation process.
Description
Technical field
The present invention relates to a kind of treatment process of refinery high density sulfur-bearing alkaline sewage, utilize the sulfide in the precipitation agent elder generation removal waste water, stench such as thioether and mercaptan class material, cut down water body toxicity, crude phenols and naphthenic acid are reclaimed in acidifying, by the organism in the electricity flocculation-Fenton reagent oxidation removal waste water, when removing most COD, improved the biodegradability of sewage then.
Background technology
In the refining of petroleum and the course of processing, for the sulfide of removing in the oil product adopts alkali washing process usually, in the process of alkali cleaning, can produce the various alkaline sewages that contain high density sulfide and hardly degraded organic substance, the quantity discharged of its CODcr, sulfide and phenol is all up to the 30%-40% of refinery gross contamination emission, along with the day by day raising of people to environmental requirement, how to finish the harmless treatment of alkaline sewage cost-effectively, become the urgent environmental issue to be solved of each refinery.Domestic refinery produces high density sulfur-bearing alkaline sewage composition and sees Table-1:
Table-1 sulfur-bearing alkaline sewage composition
Handle for this type of alkaline sewage, this alkaline residue of domestic processing generally adopts CO
2And H
2SO
4The acidifying method is carried phenol to above-mentioned alkaline residue and is proposed the pre-treatment of acid, and this technology is mature on the whole, but produces a large amount of hydrogen sulfide in acidization, causes second environmental pollution, and very big to the corrosion of equipment.Handle for alkaline sewage, the external relatively more current practice is to adopt wet oxidation process, and wet oxidation process can be divided into the Catalytic Wet Oxidation under air wet oxidation and the catalyzer condition, air wet oxidation; Can be divided into the High Temperature High Pressure wet oxidation again and relax wet oxidation according to operational condition.Wherein High Temperature High Pressure wet oxidation and Catalytic Wet Oxidation have only a small amount of application at home.What present domestic application was more is that the mitigation wet oxidation+SBR treatment process that grinds institute is comforted by China Petrochemical Industry, reach the purpose of improving the alkaline residue biodegradability by removal to most of sulfide in the alkaline residue, alkaline residue after the oxide treatment is again through the biochemical Pollutant levels that further reduce of SBR, enter oil-containing sewage treatment system at last again and carry out advanced treatment, the main mode of treatment technology is activated sludge process and deriving technology (catalytic oxidation, oxidation ditch etc.) thereof.
Chinese patent CN 1257047A adopts intermittent type biological treatment (SBR), and the salts contg that requires control SBR water inlet is less than below the 30g/L, and the water inlet volumetric loading is at 3.0KgCOD/ (m
3D) below, can obtain the stable treated effect, the concentration of alkaline sewage drops to below the 400mg/L from 1000-7000mg/L, and volatile phenol is reduced to below the 15mg/L from 400-1600mg/L.Existing alkaline sewage saltness is generally about 250-350g/L, by the requirement of the salts contg of SBR technology water inlet less than 30g/L, waste water needs to dilute more than 10 times at least, this technology not only requires Macrodilution water, the toxic problem of unresolved alkaline residue simultaneously, and be not suitable for the processing of the oil refining alkaline residue of high density.
Osaka, Japan gas Co., Ltd. has proposed a kind of wet oxidation and has handled the combined process of handling with anaerobe digestion and/or aerobe in Chinese patent CN 1050012A, solved the final problem of outlet of alkaline residue.Be characterized in that most organic is oxidized, the residual active sludge that aerobic treatment produces enters the oxidation of wet oxidation unit, and whole process is not arranged residual active sludge, and the main drawback of this method is that device working cost and investment are very expensive.
At present, prior art does not obtain good treatment effect to this type of waste water, its water outlet COD content height, the colourity height, smell is heavy, the toxicity height, enter the treatment effect that has a strong impact on the comprehensive wastewater treatment station behind the comprehensive wastewater treatment station, though perhaps water outlet COD can be reduced to below the 1000mg/L, the volume of water outlet is ten times even 20 times of former volume of water, wastewater flow rate increases greatly, does not meet the policy of energy-saving and emission-reduction.
But in order to improve the treatment effect of alkaline sewage, for refinery provides brand-new sewage solution, the problem that particularly big at the investment of present alkaline residue treatment process, narrow application range, poor processing effect, water outlet biodegradability difference etc. exist has proposed feasible, economic, solution efficiently.
Summary of the invention
The technical problem that solves: for solving the problem that present high density sulfur-bearing alkaline sewage exists, the method that the object of the present invention is to provide a kind of high density sulfur-bearing alkaline sewage to handle.
Technical scheme of the present invention is achieved in that a kind of treatment process of high density sulfur-bearing alkaline sewage, comprises following step:
The alkaline sewage of the high density sulfur-bearing that (1) refinery is come out enters settling tank, adds precipitation agent in settling tank, carries out the chemical precipitation reaction, and aeration agitation;
(2) waste water after settling tank comes out enters acidifying system recoveries crude phenols and naphthenic acid;
(3) waste water that comes out from the acidifying system, enter electric flocculation reactor and carry out electrolytic reaction, soluble anode is through hydrolysis, polymerization, produce pollutent flocculation group, pollutent flocculation group floats to the water surface by the hydrogen microbubble absorption that produces on precipitated oxygen microbubble and the negative electrode on the anode, makes it solid-liquid separation;
(4) through the waste water after the electricity flocculation, enter chemical oxidation pond and carry out Fenton (Fenton) oxidizing reaction.
In the such scheme:
Sulphur content is greater than 500mg/L in the described sulfur-bearing alkaline sewage, and COD concentration is 30000-600000mg/L, and colourity is 10000-50000 times.
The described precipitation agent of above-mentioned steps (1) is the inorganic copper-containing compound of cupric oxide, copper hydroxide or copper sulfate; The throw out that is produced reclaims by the calcining back.
Described acidifying system recoveries crude phenols and naphthenic acid, add the vitriol oil at the static mixing groove and carry out acidification, at first adjust pH to 5.0～6.0 enter water-and-oil separator, and the residence time is 2～6h, reclaim crude phenols, sour water advances the static mixing groove and continues the enriching sulfuric acid acidation, and adjust pH to 2.0～4.0 enter water-and-oil separator, the residence time is 2～6h, reclaims naphthenic acid.
Electrode in the electricity flocculation reaction is the soluble iron electrode, on electric flocculation reactor surface machinery is housed and scrapes the bubble machine.
The described Fenton of above-mentioned steps (4) (Fenton) oxidizing reaction, the Fenton oxidizing reaction is pH=2.8～5.5 just, and oxidation time is 2～5 hours, uses Ca (OH) again
2After transferring PH to be 9.0, aeration 1 hour.
Beneficial effect:
1, precipitation agent of the present invention can recycle, and has reduced running cost.
2, acidifying removal process of the present invention can not produce hydrogen sulfide, does not produce secondary pollution; Obtain not sulfur-bearing, purity is than higher crude phenols and naphthenic acid.
3, the present invention compared with prior art need not add Macrodilution water, and each section can both reduce the toxicity and the COD value of alkaline residue sewage targetedly; Go biochemical treatment system not to be impacted.
4, the waste water after the present invention handles is limpid, and volume is constant substantially, and biodegradability is good.
5, technology of the present invention is simple, and equipment investment cost is little.
6, operation and maintenance of the present invention is convenient, and stable, treatment effect is good.
Description of drawings
Fig. 1 is the process flow sheet of the treatment process of refinery high density sulfur-bearing alkaline residue of the present invention.
Embodiment
Below the present invention is described in further detail by the example example.
Embodiment 1
Sewage source is a certain refinery catalytic gasoline alkaline sewage, COD 456300mg/L wherein, and sulfide 23500mg/L, volatile phenol 93560mg/L, colourity is got catalytic gasoline alkaline sewage 2m greater than 37000 times
3Add precipitation agent copper sulfate, the mol ratio of precipitation agent and sulfide is 1.00: 1.00, aeration agitation 60 minutes is 3 hours when alkaline sewage residence time in settling tank, and sulfides from wastewater is 300mg/L, clearance reaches 98.8%, colourity has clear improvement, and toxicity reduces, residual Cu=0.01mg/L.The throw out main component that produces is CuS, generates CuO by calcining the back, but CuO direct reuse or generate CuSO through sulfuric acid acidation
4After reuse again.
Waste water after settling tank comes out enters acidification pool, transfers PH=5.3 with the vitriol oil, leaves standstill 5 hours, obtains the not crude phenols of sulfur-bearing, and the waste water COD after the dephenolize is reduced to 28500mg/L; Dephenolize waste water flows into electric flocculation reactor, and the electrode in the electric flocculation reactor is the soluble iron electrode, on electric flocculation reactor surface machinery is housed and scrapes the bubble machine, and it is 10A that strength of current is set, and the alternating impulse cycle is 45s, and electrolysis time is 2 hours.
Soluble anode is through hydrolysis, polymerization, flocculation agents such as a series of multinuclear carboxylic acid complexing ions and oxyhydroxide have been produced, while precipitated oxygen microbubble on anode, on negative electrode, produce the hydrogen microbubble, polymer organic pollutant, suspended substance and toxic substances etc. in this flocculation agent and the waste water carry out throwing out and form pollutent flocculation group, the pollutent flocculation group that produces in this oxygen and the hydrogen microbubble planar water floats to the water surface, produce the air supporting effect, scrape the bubble machine by machinery the flocculation group that is raised to above the water surface is blown off, reach the effect of solid-liquid separation; Simultaneously, oxygenants such as OH that produces in the wastewater electrolytic process and oxygen can be oxidized to larger molecular organics small organic molecule, improve the biodegradability of waste water, and the Fe that produces in anodic dissolution processes
2+And Fe
3+, for Fenton reagent provides iron ion; After this process processing, most of organism is removed in the waste water.The scum silica frost that produces is done security landfill and is handled after dehydration.
Be reduced to 12500mg/L through the waste water COD after the electricity flocculation; The back flows into the Fenton reagent oxidation pond, and the actual amount of hydrogen peroxide is 0.85: 1.00 with the ratio of theoretical consumption in the Fenton reagent, and the Fenton oxidizing reaction is pH=3.5 just, and oxidation time is 3 hours.Use Ca (OH) again
2After transferring PH to be 9.0, aeration 1 hour makes Fe (OH)
2Be converted into Fe (OH)
3Water outlet is limpid, and odorlessness, water outlet volume are 1.90m
3, COD
Cr=1650mg/L, sulfide=0.00mg/L, Cu=0.2mg/L, colourity is 3 times, BOD/COD=0.56, wastewater biodegradability is greatly improved.
Embodiment 2:
Sewage source is a certain refinery catalytic diesel oil alkaline sewage, COD 135600mg/L wherein, and sulfide 12965mg/L, volatile phenol 9765mg/L, naphthenic acid 4.5%, colourity is got catalytic diesel oil alkaline sewage 20m greater than 45000 times
3Add regeneration precipitation agent cupric oxide, the mol ratio of precipitation agent and sulfide is 1.40: 1.00, aeration agitation 90 minutes is 2 hours when alkaline sewage residence time in settling tank, and sulfides from wastewater is 77.8mg/L, clearance reaches 99.4%, colourity has clear improvement, and toxicity reduces, residual Cu=1.20mg/L; Acidification pool is removed in water outlet, transfers pH value to 5.7 with the vitriol oil, leaves standstill 3 hours, reclaims crude phenols, is acidified to pH value 3.3 again, leaves standstill 3 hours, and layering obtains the not naphthenic acid of sulfur-bearing, and this moment, waste water COD was reduced to 35400mg/L; Back waste water flows into electric flocculation reactor, and it is 15A that strength of current is set, and the alternating impulse cycle is 60s, and electrolysis time is 3 hours, and waste water COD is reduced to 16300mg/L; The back flows into the Fenton reagent oxidation pond, and the actual amount of hydrogen peroxide is 1.10: 1.00 with the ratio of theoretical consumption in the Fenton reagent, and the Fenton oxidizing reaction is pH=4.5 just, and oxidation time is 4 hours.Use Ca (OH) again
2After transferring PH to be 9.0, aeration 1 hour makes Fe (OH)
2Be converted into Fe (OH)
3Water outlet is limpid, and odorlessness, water outlet volume are 18.5m
3, COD
Cr=1810mg/L, sulfide=0.00mg/L, Cu=0.15mg/L, colourity is 3 times, BOD/COD=0.62, wastewater biodegradability is greatly improved.
Embodiment 3
Sewage source is a certain refinery catalytic diesel oil alkaline sewage, COD 30000mg/L wherein, and sulfide 8000mg/L, volatile phenol 9765mg/L, naphthenic acid 4.5%, colourity is got catalytic diesel oil alkaline sewage 20m greater than 10000 times
3, adding regeneration precipitation agent cupric oxide, the mol ratio of precipitation agent and sulfide is 0.6: 1.00, and aeration agitation 30 minutes is 1 hour when alkaline sewage residence time in settling tank, and sulfides from wastewater is 40mg/L, and colourity has clear improvement, and toxicity reduces.
Acidification pool is removed in water outlet, transfers pH value to 5.0 with the vitriol oil, leaves standstill 2 hours, reclaim crude phenols, be acidified to pH value 2.0 again, left standstill 2 hours, layering obtains the not naphthenic acid of sulfur-bearing, and back waste water flows into electric flocculation reactor, and it is 15A that strength of current is set, the alternating impulse cycle is 60s, electrolysis time is 3 hours, and the back flows into the Fenton reagent oxidation pond, and the actual amount of hydrogen peroxide is 0.50: 1.00 with the ratio of theoretical consumption in the Fenton reagent, the Fenton oxidizing reaction is pH=2.8 just, and oxidation time is 2 hours.Use Ca (OH) again
2After transferring PH to be 9.0, aeration 1 hour makes Fe (OH)
2Be converted into Fe (OH)
3Water outlet is limpid, odorlessness.
Embodiment 4
Sewage source is a certain refinery catalytic diesel oil alkaline sewage, COD 600000mg/L wherein, and sulfide 18000mg/L, volatile phenol 9765mg/L, naphthenic acid 4.5%, 50000 times of colourities are got catalytic diesel oil alkaline sewage 20m
3, adding regeneration precipitation agent cupric oxide, the mol ratio of precipitation agent and sulfide is 1.6: 1.00, and aeration agitation 120 minutes is 4 hours when alkaline sewage residence time in settling tank, and sulfides from wastewater is 90mg/L, and colourity has clear improvement, and toxicity reduces.
Acidification pool is removed in water outlet, transfers pH value to 6.0 with the vitriol oil, leaves standstill 6 hours, reclaim crude phenols, be acidified to pH value 4.0 again, left standstill 6 hours, layering obtains the not naphthenic acid of sulfur-bearing, and back waste water flows into electric flocculation reactor, and it is 15A that strength of current is set, the alternating impulse cycle is 60s, electrolysis time is 3 hours, and the back flows into the Fenton reagent oxidation pond, and the actual amount of hydrogen peroxide is 1.30: 1.00 with the ratio of theoretical consumption in the Fenton reagent, the Fenton oxidizing reaction is pH=5.5 just, and oxidation time is 5 hours.Use Ca (OH) again
2After transferring PH to be 9.0, aeration 5 hours makes Fe (OH)
2Be converted into Fe (OH)
3Water outlet is limpid, odorlessness.
Claims (6)
1. the treatment process of a refinery high density sulfur-bearing alkaline sewage is characterized in that may further comprise the steps:
The alkaline sewage of the high density sulfur-bearing that (1) refinery is come out enters settling tank, adds precipitation agent in settling tank, carries out the chemical precipitation reaction, and aeration agitation;
(2) waste water after settling tank comes out enters acidifying system recoveries crude phenols and naphthenic acid;
(3) waste water that comes out from the acidifying system, enter electric flocculation reactor and carry out electrolytic reaction, soluble anode is through hydrolysis, polymerization, produce pollutent flocculation group, the hydrogen microbubble absorption that the pollutent flocculation is rolled into a ball by producing on oxygen microbubble of separating out on the anode and the negative electrode floats to the water surface, makes it solid-liquid separation;
(4) through the waste water after the electricity flocculation, enter chemical oxidation pond and carry out Fenton (Fenton) oxidizing reaction.
2. the treatment process of a kind of refinery high density sulfur-bearing alkaline residue according to claim 1 is characterized in that: sulfide is greater than 500mg/L in the described sulfur-bearing alkaline sewage, and COD concentration is 30000-600000mg/L, and colourity is 10000-50000 times.
3. the treatment process of a kind of refinery high density sulfur-bearing alkaline sewage according to claim 1 is characterized in that: the described precipitation agent of step (1) is the inorganic copper-containing compound of cupric oxide, copper hydroxide or copper sulfate; The throw out that is produced reclaims by the calcining back.
4. the treatment process of a kind of refinery high density sulfur-bearing alkaline sewage according to claim 1, it is characterized in that: described acidifying system recoveries crude phenols and naphthenic acid add the vitriol oil at the static mixing groove and carry out acidification, at first adjust pH to 5.0～6.0, enter water-and-oil separator, the residence time is 2～6 hours, reclaims crude phenols, and sour water advances the static mixing groove and continues the enriching sulfuric acid acidation, adjust pH to 2.0～4.0, enter water-and-oil separator, the residence time is 2～6 hours, reclaims naphthenic acid.
5. the treatment process of a kind of refinery high density sulfur-bearing alkaline sewage according to claim 1 is characterized in that: the electrode in the electric flocculation reactor is the soluble iron electrode, on electric flocculation reactor surface machinery is housed and scrapes the bubble machine.
6. the treatment process of a kind of refinery high density sulfur-bearing alkaline sewage according to claim 1, it is characterized in that: the described Fenton of step (4) (Fenton) oxidizing reaction, the Fenton oxidizing reaction is pH=2.8～5.5 just, and oxidation time is 2～5 hours, uses Ca (OH) again
2After transferring PH=9.0, aeration 1 hour.
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