CN101264996B - Method for treating aniline waste water by absorption-low temperature dry method - Google Patents
Method for treating aniline waste water by absorption-low temperature dry method Download PDFInfo
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- CN101264996B CN101264996B CN2008100548326A CN200810054832A CN101264996B CN 101264996 B CN101264996 B CN 101264996B CN 2008100548326 A CN2008100548326 A CN 2008100548326A CN 200810054832 A CN200810054832 A CN 200810054832A CN 101264996 B CN101264996 B CN 101264996B
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Abstract
A low temperature dry treatment method of aniline wastewater by adsorption comprises the steps of feeding aniline wastewater into a fixed-bed reactor filled with adsorption-catalyst until the anilineconcentration in the effluent wastewater after adsorption is 4.9 mg/L, discharging residual water in the reactor, introducing oxidizing gas with oxygen volumetric concentration of 4-6% and air speed of 500-2,000 h<-1>, reacting at 100-400 DEG C for 1-10 hours, and using the adsorption-catalyst after catalytic oxidation on the next stage of adsorption-catalytic oxidation. The inventive method can efficiently remove aniline pollutant from wastewater; and has the advantages of no secondary pollution, reusability of adsorption-catalyst, and low cost.
Description
Technical field
The invention belongs to a kind of method for the treatment of aniline waste water by absorption-low temperature dry method.
Background technology
Aniline is one of important intermediate of chemical industry, is used in a large number in the production of dyestuff, agricultural chemicals, rubber ingredients, urethane foam, and aniline content is higher in the waste water of these enterprise's dischargings.Aniline has high toxicity, carinogenicity and difficult degradation to biology, and the EPA of U.S. environment administration classifies aniline as priority pollutants.All there are strict restriction in developed country and China to aniline content in the waste water of production plant.China waste water III level emission standard is 5mg/L.
At present, the adsorption technology based on the good absorption property of gac has a wide range of applications at organic waste water and off gas treatment field.With gac as sorbent material can effectively handle VOCs in the waste gas and waste water aniline (charcoal, 2004 .42:653-665., colloid and surfaces A, 2005,265:32-39), visible gac has the good adsorption performance to this type organic.But after in a single day the loading capacity of gac reaches capacity, just need handle so that utilize again it.Regeneration techniques commonly used is heat regeneration in the industry at present.In the hot regenerative process, the gac that adsorbs after saturated will be handled under 800-850 ℃ high temperature, and energy consumption is big; Simultaneously, high-temperature operation makes that the loading capacity rate of loss of gac is big, a charcoal absorption capacitance loss of every regeneration 5-15%; In addition, high-temperature operation also makes gac need specific regenerating unit regeneration, thereby increases stevedore charge and can cause a certain amount of gac loss in transportation; And aniline and other pollutents of desorption also needs aftertreatment, complex process in the regenerative process.
Summary of the invention
The object of the present invention is to provide a kind of active height, the method for the simple treating aniline waste water by absorption-low temperature dry method of technology.
On gac, support a certain amount of metal oxide and make metal/charcoal (AC) absorption-catalyzer, utilize the good absorption property of gac to purify liquid waste, pollutent is concentrated, drain in the reactor behind the residual water, be blown into oxidizing gas, utilize the catalytic activity and the selectivity of catalyzer, under mild conditions, adsorbed contaminants is degraded to CO
2, H
2O and N
2Thereby, absorption-catalyzer is regenerated.Absorption-low temperature dry method catalytic oxidation is a kind of feasible and cost-effective method of wastewater treatment.
Absorption-catalyzer provided by the invention contains a kind of among transition metal Cu, Fe, Co and the Ni, and it is to be carrier with the gac, and the weight percent of its component is: metal 1-10%, gac are 90-99%, and the surface-area of gac is 500-1500m
2/ g.The preparation method is: behind the nitrate incipient impregnation carrier active carbon with Cu, Fe, Co and Ni, left standstill under the room temperature 2-4 hour, at 50-110 ℃ of dry 6-16 hour, calcining got final product in 2-4 hour under 200-500 ℃ of inert atmosphere then.Concrete summary of the invention see publication number CN1792441A's " a kind of processing wastewater containing phenol absorption-catalyzer and method for making and application ".
Charcoal base absorption-Application of Catalyst method provided by the invention will be for will contain aniline waste water by the fixed-bed reactor of this absorption-catalyzer are housed, when the aniline concentration in the waste water that discharge the absorption back equals 4.9mg/L, stop into water, the residual water in the reactor of draining, the aerating oxygen volumetric concentration is the oxidizing gas of 4-6% then, and air speed is 500-2000h
-1, temperature of reaction is 100-400 ℃, reaction 1-10h, and behind catalytic oxidation process, absorption-catalyzer is used for next absorption-catalyzed oxidation working cycle.
Aforesaid oxidizing gas is the mixed gas by oxygen and nitrogen, or the mixed gas of air and nitrogen, or the mixed gas of oxygen and argon gas, or the mixed gas of air and argon gas.
The present invention has compared following advantage with prior art:
1. charcoal base absorption-catalyzer has good absorption property, can remove pollutent such as aniline in the waste water efficiently.
2. catalyzed oxidation mild condition, oxidation under the low-temperature atmosphere-pressure need not a large amount of water body heating and pressurizing, and energy consumption is low, and occupation area of equipment is little, process and simple to operate, catalyzed oxidation on the throne can change into CO with the aniline Catalytic Oxygen
2, H
2O and N
2, do not produce secondary pollution.Waste water after the processing can reuse, has saved a large amount of process waters.
3. charcoal base absorption-catalyzer can use behind catalyzed oxidation continuously, and cost is low.
Embodiment
Embodiment 1
The Cu5/AC Preparation of catalysts
With 100g 40-60 order specific surface area is 1000m
2The gac of/g, join in the copper nitrate solution of 100ml 0.78mol/L, stirred, room temperature was placed 4 hours, and in 80 ℃ of oven dry 9 hours, calcining was 3 hours under 300 ℃ of inert atmospheres, naturally cool to room temperature and make catalyst A, the weight of the metal component in the catalyzer is: Cu5%, gac 95% is labeled as Cu5/AC.
The use of Cu5/AC absorption-catalyzer
(the carrier active carbon specific surface area is 1000m will to contain the adsorption column of 1000mg/L aniline waste water 50ml by 0.5g Cu5 (wt%) absorption-catalyzer is housed
2/ g), when the aniline concentration in the waste water that discharge the absorption back equals 4.9mg/L, stop into water, residual water in the reactor of draining, giving aerating oxygen volumetric concentration in Cu5 (wt%) the charcoal base absorption-catalyzer is 4% the mixed gas of being made up of oxygen and nitrogen, and air speed is 1000h
-1, and temperature risen to 200 ℃; 200 ℃ of following constant temperature catalyzed oxidations 10 hours.Catalyzed oxidation reduces the temperature to room temperature after finishing in oxidizing atmosphere.
Experimental result: the aniline in the waste water can get 99% removal, Cu5 after the regeneration (wt%) absorption-catalyzer can adsorb 50ml once more and contain in the 1000mg/L aniline waste water 98% aniline, online mass spectrometric detection repeatedly in the working cycle pollutent catalyzing oxidizing degrading product be CO
2, H
2O and N
2
Embodiment 2
The Cu10/AC Preparation of catalysts
With 100g 40-60 order specific surface area is 1500m
2The gac of/g, join in the copper nitrate solution of 100ml 1.56mol/L, stirred, room temperature was placed 3 hours, and in 110 ℃ of oven dry 16 hours, calcining was 4 hours under 500 ℃ of inert atmospheres, naturally cool to room temperature and make catalyst B, the weight of the metal component in the catalyzer is: Cu10%, gac 90% is labeled as Cu10/AC.
The use of Cu10/AC absorption-catalyzer
(the carrier active carbon specific surface area is 1500m will to contain the adsorption column of 1500mg/L aniline waste water 50ml by 0.5g Cu 10 (wt%) absorption-catalyzer is housed
2/ g), when the aniline concentration in the waste water that discharge the absorption back equals 4.9mg/L, stop into water, residual water in the reactor of draining, giving aerating oxygen volumetric concentration in Cu 10 (wt%) the charcoal base absorption-catalyzer is 5% the mixed gas of forming by air and nitrogen, and air speed is 2000h
-1, and temperature risen to 400 ℃; 400 ℃ of following constant temperature catalyzed oxidations 8 hours.Catalyzed oxidation reduces the temperature to room temperature after finishing in oxidizing atmosphere.
Experimental result: the aniline in the waste water can get 99% removal, Cu 10 (wt%) absorption-catalyzer after the regeneration can adsorb 50ml once more and contain in the 1500mg/L aniline waste water 97% aniline, online mass spectrometric detection repeatedly in the working cycle pollutent catalyzing oxidizing degrading product be CO
2, H
2O and N
2
Embodiment 3
The Fe3/AC Preparation of catalysts
With 100g 40-60 order specific surface area is 500m
2The gac of/g, join in the iron nitrate solution of 100ml 0.536mol/L, stirred, room temperature was placed 2 hours, and in 50 ℃ of oven dry 7 hours, calcining was 2 hours under 400 ℃ of inert atmospheres, naturally cool to room temperature and make catalyzer C, the weight of the metal component in the catalyzer is: Fe3%, gac 97% is labeled as Fe3/AC.
The use of Fe3/AC absorption-catalyzer
(the carrier active carbon specific surface area is 500m will to contain the adsorption column of 500mg/L aniline waste water 50ml by 0.5g Fe3 (wt%) absorption-catalyzer is housed
2/ g), when the aniline concentration in the waste water that discharge the absorption back equals 4.9mg/L, stop into water, residual water in the reactor of draining, giving aerating oxygen volumetric concentration in Fe3 (wt%) the charcoal base absorption-catalyzer is 6% the mixed gas of being made up of oxygen and argon gas, and air speed is 500h
-1, and temperature risen to 250 ℃; 250 ℃ of following constant temperature catalyzed oxidations 4 hours.Catalyzed oxidation reduces the temperature to room temperature after finishing in oxidizing atmosphere.
Experimental result: the aniline in the waste water can get 99% removal, Fe3 after the regeneration (wt%) absorption-catalyzer can adsorb 50ml once more and contain in the 500mg/L aniline waste water 97% aniline, online mass spectrometric detection repeatedly in the working cycle pollutent catalyzing oxidizing degrading product be CO
2, H
2O and N
2
Embodiment 4
The Fe8/AC Preparation of catalysts
With 100g 40-60 order specific surface area is 1500m
2The gac of/g, join in the copper nitrate solution of 100ml1.429mol/L, stirred, room temperature was placed 3 hours, and in 100 ℃ of oven dry 12 hours, calcining was 2 hours under 400 ℃ of inert atmospheres, naturally cool to room temperature and make catalyzer D, the weight of the metal component in the catalyzer is: Fe8%, gac 92% is labeled as Fe8/AC.
The use of Fe8/AC absorption-catalyzer
(the carrier active carbon specific surface area is 1500m will to contain the adsorption column of 1500mg/L aniline waste water 50ml by 0.5g Fe8 (wt%) absorption-catalyzer is housed
2/ g), when the aniline concentration in the waste water that discharge the absorption back equals 4.9mg/L, stop into water, residual water in the reactor of draining, giving aerating oxygen volumetric concentration in Fe8 (wt%) the charcoal base absorption-catalyzer is 4% the mixed gas of being made up of air and argon gas, and air speed is 1500h
-1, and temperature risen to 400 ℃; 400 ℃ of following constant temperature catalyzed oxidations 8 hours.Catalyzed oxidation reduces the temperature to room temperature after finishing in oxidizing atmosphere.
Experimental result: the aniline in the waste water can get 99% removal, Fe8 after the regeneration (wt%) absorption-catalyzer can adsorb 50ml once more and contain in the 1500mg/L aniline waste water 98% aniline, online mass spectrometric detection repeatedly in the working cycle pollutent catalyzing oxidizing degrading product be CO
2, H
2O and N
2
Embodiment 5
The Co4/AC Preparation of catalysts
With 100g 40-60 order specific surface area is 500m
2The gac of/g, join in the copper nitrate solution of 100ml 0.678mol/L, stirred, room temperature was placed 2 hours, and in 50 ℃ of oven dry 16 hours, calcining was 3 hours under 200 ℃ of inert atmospheres, naturally cool to room temperature and make catalyzer E, the weight of the metal component in the catalyzer is: Co4%, gac 96% is labeled as Co4/AC.
The use of Co4/AC absorption-catalyzer
(the carrier active carbon specific surface area is 500m will to contain the adsorption column of 500mg/L aniline waste water 50ml by 0.5g Co4 (wt%) absorption-catalyzer is housed
2/ g), when the aniline concentration in the waste water that discharge the absorption back equals 4.9mg/L, stop into water, residual water in the reactor of draining, giving aerating oxygen volumetric concentration in Co4 (wt%) the charcoal base absorption-catalyzer is 5% the mixed gas of being made up of oxygen and nitrogen, and air speed is 500h
-1, and temperature risen to 260 ℃; 260 ℃ of following constant temperature catalyzed oxidations 8 hours.Catalyzed oxidation reduces the temperature to room temperature after finishing in oxidizing atmosphere.
Experimental result: the aniline in the waste water can get 99% removal, Co4 after the regeneration (wt%) absorption-catalyzer can adsorb 50ml once more and contain in the 500mg/L aniline waste water 98% aniline, online mass spectrometric detection repeatedly in the working cycle pollutent catalyzing oxidizing degrading product be CO
2, H
2O and N
2
Embodiment 6
The Co7/AC Preparation of catalysts
With 100g 40-60 order specific surface area is 1500m
2The gac of/g, join in the copper nitrate solution of 100ml1.187mol/L, stirred, room temperature was placed 3 hours, and in 110 ℃ of oven dry 10 hours, calcining was 4 hours under 350 ℃ of inert atmospheres, naturally cool to room temperature and make catalyzer C, the weight of the metal component in the catalyzer is: Co7%, gac 93% is labeled as Co7/AC.
The use of Co7/AC absorption-catalyzer
(the carrier active carbon specific surface area is 1500m will to contain the adsorption column of 1500mg/L aniline waste water 50ml by 0.5g Co7 (wt%) absorption-catalyzer is housed
2/ g), when the aniline concentration in the waste water that discharge the absorption back equals 4.9mg/L, stop into water, residual water in the reactor of draining, giving aerating oxygen volumetric concentration in Co7 (wt%) the charcoal base absorption-catalyzer is 6% the mixed gas of being made up of air and nitrogen, and air speed is 1500h
-1, and temperature risen to 400 ℃; 400 ℃ of following constant temperature Catalytic Oxygen 6 hours.Catalyzed oxidation reduces the temperature to room temperature after finishing in oxidizing atmosphere.
Experimental result: the aniline in the waste water can get 99% removal, Co7 after the regeneration (wt%) absorption-catalyzer can adsorb 50ml once more and contain in the 1500mg/L aniline waste water 97.5% aniline, online mass spectrometric detection repeatedly in the working cycle pollutent catalyzing oxidizing degrading product be CO
2, H
2O and N
2
Embodiment 7
The Ni1/AC Preparation of catalysts
With 100g 40-60 order specific surface area is 500m
2The gac of/g, join in the copper nitrate solution of 100ml 0.170mol/L, stirred, room temperature was placed 4 hours, and in 70 ℃ of oven dry 9 hours, calcining was 3 hours under 300 ℃ of inert atmospheres, naturally cool to room temperature and make catalyzer G, the weight of the metal component in the catalyzer is: Ni1%, gac 99% is labeled as Ni1/AC.
The use of Ni1/AC absorption-catalyzer
(the carrier active carbon specific surface area is 500m will to contain the adsorption column of 500mg/L aniline waste water 50ml by 0.5g Ni1 (wt%) absorption-catalyzer is housed
2/ g), when the aniline concentration in the waste water that discharge the absorption back equals 4.9mg/L, stop into water, residual water in the reactor of draining, giving aerating oxygen volumetric concentration in Ni1 (wt%) the charcoal base absorption-catalyzer is 4% the mixed gas of being made up of oxygen and argon gas, and air speed is 500h
-1, and temperature risen to 200 ℃; 200 ℃ of following constant temperature catalyzed oxidations 10 hours.Catalyzed oxidation reduces the temperature to room temperature after finishing in oxidizing atmosphere.
Experimental result: the aniline in the waste water can get 99% removal, Ni1 after the regeneration (wt%) absorption-catalyzer can adsorb 50ml once more and contain in the 500mg/L aniline waste water 97% aniline, online mass spectrometric detection repeatedly in the working cycle pollutent catalyzing oxidizing degrading product be CO
2, H
2O and N
2
Embodiment 8
The Ni10/AC Preparation of catalysts
With 100g 40-60 order specific surface area is 1500m
2The gac of/g, join in the copper nitrate solution of 100ml 1.70mol/L, stirred, room temperature was placed 2 hours, and in 110 ℃ of oven dry 10 hours, calcining was 4 hours under 500 ℃ of inert atmospheres, naturally cool to room temperature and make catalyzer H, the weight of the metal component in the catalyzer is: Ni10%, gac 90% is labeled as Ni10/AC.
The use of Ni10/AC absorption-catalyzer
(the carrier active carbon specific surface area is 1500m will to contain the adsorption column of 1500mg/L aniline waste water 50ml by 0.5g Ni10 (wt%) absorption-catalyzer is housed
2/ g), when the aniline concentration in the waste water that discharge the absorption back equals 4.9mg/L, stop into water, residual water in the reactor of draining, giving aerating oxygen volumetric concentration in Ni10 (wt%) the charcoal base absorption-catalyzer is 5% the mixed gas of being made up of air and argon gas, and air speed is 2000h
-1, and temperature risen to 400 ℃; 400 ℃ of following constant temperature catalyzed oxidations 6 hours.Catalyzed oxidation reduces the temperature to room temperature after finishing in oxidizing atmosphere.
Experimental result: the aniline in the waste water can get 99% removal, Ni10 after the regeneration (wt%) absorption-catalyzer can adsorb 50ml once more and contain in the 1500mg/L aniline waste water 98% aniline, online mass spectrometric detection repeatedly in the working cycle pollutent catalyzing oxidizing degrading product be CO
2, H
2O and N
2
Claims (2)
1. the method for a treating aniline waste water by absorption-low temperature dry method is characterized in that comprising the steps:
To contain aniline waste water by the fixed-bed reactor of absorption-catalyzer are housed, when the aniline concentration in the waste water that discharge the absorption back equals 4.9mg/L, stop into water, residual water in the reactor of draining, the aerating oxygen volumetric concentration is the oxidizing gas of 4-6% then, and air speed is 500-2000h
-1, temperature of reaction is 100-400 ℃, reaction 1-10h, and behind catalytic oxidation process, absorption-catalyzer is used for next absorption-catalyzed oxidation working cycle;
Described absorption-catalyzer is to contain a kind of among transition metal Cu, Fe, Co and the Ni, is carrier with the gac, and the weight percent of its component is: transition metal 1-10%, gac are 90-99%, and the specific surface area of gac is 500-1500m
2/ g.
2. the method for a kind for the treatment of aniline waste water by absorption-low temperature dry method as claimed in claim 1 is characterized in that described oxidizing gas is the mixed gas of mixed gas, oxygen and argon gas of mixed gas, air and nitrogen of oxygen and nitrogen or the mixed gas of air and argon gas.
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| CN101264996B true CN101264996B (en) | 2010-06-02 |
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102092870B (en) * | 2010-12-31 | 2012-07-04 | 大连理工大学 | Sewage treatment equipment and process for concentration/chemical oxidation regeneration of absorbent |
| CN102249376B (en) * | 2011-05-20 | 2012-12-12 | 北京化工大学 | Method for realizing recycling of aniline waste water and zero release through electropolymerization |
| CN106007125A (en) * | 2016-07-08 | 2016-10-12 | 重庆交通大学 | Dye wastewater treatment technology |
| CN106335999A (en) * | 2016-11-10 | 2017-01-18 | 湖北君集水处理有限公司 | System and method for advanced treatment of industrial sewage |
| CN114684952B (en) * | 2020-12-31 | 2023-08-01 | 中国石油化工股份有限公司 | Method and device for treating low COD sewage |
Citations (2)
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|---|---|---|---|---|
| US5063196A (en) * | 1989-06-23 | 1991-11-05 | Calgon Carbon Corporation | Chromium-free impregnated activated carbon for adsorption of toxic gases and/or vapors |
| CN1792441A (en) * | 2005-12-21 | 2006-06-28 | 中国科学院山西煤炭化学研究所 | Adsorption-catalyst for treating phenol containing waste-water, prepn. method and application thereof |
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2008
- 2008-04-15 CN CN2008100548326A patent/CN101264996B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5063196A (en) * | 1989-06-23 | 1991-11-05 | Calgon Carbon Corporation | Chromium-free impregnated activated carbon for adsorption of toxic gases and/or vapors |
| CN1792441A (en) * | 2005-12-21 | 2006-06-28 | 中国科学院山西煤炭化学研究所 | Adsorption-catalyst for treating phenol containing waste-water, prepn. method and application thereof |
Non-Patent Citations (4)
| Title |
|---|
| H.T.Gomes.et al..Transition metal (Cu,Cr, and V) modified MCM-41 forthecatalytic wet air oxidation of aniline.Microporous and Mesoporous Materials86.2005,86287-294. * |
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