CN103979731B - A kind of method utilizing pollutent self-assembly electro-chemical systems aniline degradation waste water - Google Patents
A kind of method utilizing pollutent self-assembly electro-chemical systems aniline degradation waste water Download PDFInfo
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Abstract
The invention discloses a kind of method utilizing pollutent self-assembly electro-chemical systems aniline degradation waste water, comprise the steps: that aniline waste water is carried out short distance nitration by (1), containing nitrite in the aniline waste water after short distance nitration; (2) aniline waste water after short distance nitration is passed in electrolyzer, first carry out low voltage self-assembly; Carry out high-pressure electrolysis again; In this step, low voltage self-assembly and high-voltage electrolysis alternate cycles are carried out, and add the short distance nitration water outlet in step (1), until Aniline concentration reaches required value after each loop ends in electrolyzer.The present invention is optimized electrolytic process, utilizes the modifying process of pollutent aniline own, a large amount of aniline is self-assembled to electrode surface, improve electrode efficiency, also improve aniline and electrode contact surface simultaneously, accelerate mutual electron transmission, aniline is more easily degraded.The method only need add Trace Nitrite, and with low-voltage electrolysis, cleans low power consuming.
Description
Technical field
The present invention relates to technical field of sewage, be specifically related to a kind of method utilizing pollutent self-assembly electro-chemical systems aniline degradation waste water.
Background technology
Principal pollutant in aniline waste water are aniline and nitrogen, aniline is the most representative material of aromatic amine, it is a kind of colourless oil liquid with aromatic odour, be widely used in national defence, printing and dyeing, plastics, paint, agricultural chemicals and medicine industry etc., the objectionable impurities being simultaneously also serious environment pollution and being detrimental to health is that three of a kind of " carcinogenic, teratogenesis, mutagenesis " cause material.There is due to aniline the features such as extended residual, bioconcentration, carinogenicity, be classified as 129 kinds of pollutents of priority acccess control by U.S. EPA, be also put in " Chinese environmental priority pollutant Black List ", in industrial water drainage, require strict control.Amino benzene analog waste water has following characteristics usually: pollutent complex structure, concentration are high, saltiness is high, waste water sour (alkali) property is strong, readily biodegradable, bio-toxicity are large deeply, not for color and luster.And much aniline has been substituted halogen, such as common fluoroaniline, chloroaniline etc., the toxicity of these halo aniline and degraded difficulty far super aniline especially.Wherein aniline category matter needs because of its production process, causes ammonia nitrogen and aniline must be principal pollutant in such waste water.
Publication number is that the Chinese invention patent application of CN102936079A A discloses a kind of method removing aniline from the high saliferous aniline waste water of industry, with solvent extration under salting out, aniline waste water is processed, in normal pressure static mixing reactor, by waste water, sodium-chlor and mixing as the oil of mirbane of extraction solvent, tubular type static mixing reactor is squeezed into through feedstock pump, extraction solvent oil of mirbane is fully mixed with aniline waste water, raffinate is carried out the process of Aerobic-anaerobic microbiological oxidation combination process, raffinate stream is made to carry out anaerobic degradation process through anaerobic pond, enter Aerobic Pond through the waste water of anaerobic treatment and carry out aerobic degradation process.
Publication number is that the Chinese invention patent application document of CN100500584 discloses and combined with physical filtering process by electrolytic acid cleaning oxydation process, and physical filtering process is that electrolytic acid cleaning oxydation process reduces load, improves electrolytic efficiency; Two kinds of processes hocket; Adopt titanium base iridium system precious metal oxide coating anode, electrochemical catalytic oxidation aniline degradation in a cell, in the process of degraded, the mode of physical filtering is adopted with the timed interval of 30 ~ 60min, remove the wadding that in solution, electrolysis aniline produces and float intermediate product, reach the object of fast degradation aniline.
Patent 201110131660.X proposes a kind of method being realized aniline waste water resource utilization and zero release by electropolymerization, by the continuous polymerization of aniline polymerization film forming on stainless steel anode and film forming, consume the aniline composition in waste water, finally make aniline waste water Non-toxic, aniline polymer film forming can be used as product-collecting, appropriate residual aniline waste water can be used as the make up water of boiler recirculated water, plays biocide effect, realizes the zero release of aniline waste water.The method need add a large amount of sodium sulfate and improve conductivity of waste water, and by the index calculate provided in its invention, the highest meeting causes waste water salinity to improve 24g/L, far cannot reach emission request.And waste water desalination is difficult point maximum in wastewater treatment now, it is almost impossible for this salinity being removed.
Summary of the invention
The invention provides a kind of method utilizing electrochemical degradation phenolic waste water, first utilize short distance nitration process that a large amount of ammonia nitrogens in waste water are transformed into nitrite, nitrite aequum is few, and therefore conventional nitrosation process can meet.And then utilize the modifying process of pollutent aniline and nitrite itself, a large amount of aniline is self-assembled to electrode surface, improves electrode efficiency, also improve aniline and electrode contact surface simultaneously, accelerate mutual electron transmission, aniline is more easily degraded.
Utilize a method for pollutent self-assembly electro-chemical systems aniline degradation waste water, it is characterized in that, comprise the steps:
(1) aniline waste water is carried out short distance nitration, containing nitrite in the aniline waste water after short distance nitration;
(2) aniline waste water after short distance nitration is passed in electrolyzer, first carry out low voltage self-assembly; Carry out high-pressure electrolysis again; In this step, low voltage self-assembly and high-voltage electrolysis alternate cycles are carried out, and add the short distance nitration water outlet in step (1), until Aniline concentration reaches required value after each loop ends in electrolyzer.
In the aniline waste water of the inventive method process, itself is containing nitrogen salt, short distance nitration described in step (1) is the conventional short distance nitration in this area, normal containing nitrogen salt in general aniline waste water, be transformed into nitrite after carrying out conventional short distance nitration, in this wastewater degradation process, then can directly utilize the nitrite originally contained in waste water to carry out self-assembly.The present invention is optimized electrolytic process, pollutent aniline itself and nitrite is utilized to react, amino on phenyl ring is departed from, originally connected the carbon atom then active increase of amine groups, this carbon atom very easily connects hydroxyl or is connected on Graphite Electrodes, the phenyl ring connecting hydroxyl is phenol, and phenol is easily by open loop chain rupture; And self-assemble to the phenyl ring of electrode surface, then owing to improve phenyl ring and electrode contact area, therefore accelerate mutual electron transmission, phenyl ring is more easily degraded, in addition, aniline category matter is modified to the performance that electrode surface can also improve electrode; The aniline of also non-diazonium salt reaction in the solution then still traditionally electrolytic acid cleaning oxydation process degraded simultaneously.Three paths simultaneously aniline degradation thus the efficient performance improving electrochemical degradation.
As preferably, step (2) is at every turn in circulation: low voltage is 1 ~ 2V, and the self-assembly time is 2 ~ 5h; High-voltage is 4 ~ 6V, and electrolysis time is 0.2 ~ 0.5h.
In low-voltage electrolysis process, control voltage is 1 ~ 2V, and brownout has then been difficult to modified effect, and overtension then causes aniline category matter will be degraded in the solution, and the material being modified to electrode surface is less, and power consumption greatly.High-pressure electrolysis control voltage is at 4 ~ 6V, and brownout, the material of electrode surface is difficult to be sufficiently damaged, and overtension then also has comparatively havoc to graphite itself, and power consumption greatly.It is poor that nitrite combined amount crosses modified effect at least, crosses and cause waste water concentration of aniline again to rise at most, affect W-response.
More preferably, during step (2) circulates at every turn: low voltage is 1.5V, and the self-assembly time is 3h; High-voltage is 5V, and electrolysis time is 0.2h.As preferably, the aniline waste water carrying out short distance nitration described in step (1) is the waste water that specific conductivity is less than 1ms/cm.The too high waste water of specific conductivity belongs to high-salt wastewater electrolysis field, can high cost process fast by indirect oxidation or direct oxidation.Low conductivity then conventional electrolysis efficiency is low even to no effect.
As preferably, in working cycle, waste water ph controls is 7 ~ 7.5.PH7 ~ 8 are best suited for the pH of short distance nitration, and the optimum pH of self-assembly is 5 ~ 7.5, and therefore for reaching best degraded pH, and save acid-base reagent expense, selection pH is 7 ~ 7.5.
As preferably, in step (2) first time circulation time, waste water nitrite desired concn >1mM/L.I.e. step (1) medium or short range nitrified effluent nitrite concentration >1mM/L.
As preferably, circulate the beginning from second time, the short distance nitration water outlet at every turn added is by 1cm
2just to the nitrite amount needed for electrode area 1mM aniline be 0.02-0.2mM/ (Lh) calculate.
In this technological process, need measure the nitrite amount of short distance nitration process water outlet, then calculate mixing nitrosification water outlet according to above-mentioned aequum, because nitrite aequum is extremely low, therefore the wastewater flow rate of new mixing is few, can not produce large impact to overall concentration of aniline.
As preferably, the reaction electrode spacing in described electrolyzer is 2cm-10cm.
Further preferably, the combination of above-mentioned preferred version is selected.
Method of the present invention also can process the amino benzene analog waste water of the nonnitrogenous salt of minority, then select the solid nitrite adding aequum in working cycle in addition.
As preferably, the anode in described electrolyzer is graphite cake, graphite rod, carbon felt, one or several in carbon paper or graphite granule; Negative electrode in described electrolyzer is graphite cake, graphite rod, carbon felt, one or several in carbon paper or graphite granule.
Further preferably, described anode is graphite anode: negative electrode is graphite cathode, and graphite anode and graphite cathode area ratio are 5 ~ 100.
Electrode in electrolytic process selects Graphite Electrodes, and only have noble electrode surface to be just modified upper aniline category matter, in addition, Graphite Electrodes is comparatively honest, can reduce costs at electrolytic process.
The specific surface area of graphite anode much larger than graphite cathode, because modification generation anode, so need can improve modification efficiency.
Most preferably, anode adopts cylindrical graphite plate, and negative electrode adopts graphite rod, and controlling wastewater pH in degradation process is 7, and low pressure is 2V, and electrolysis time is 3h, and high pressure is 6V, electrolysis 0.2h, and recycling waste water nitrite concentration is 2mM/L for the first time; Circulate the beginning from second time, the short distance nitration water outlet at every turn added is by 1cm
2just to the nitrite amount needed for electrode area 3mM aniline be 0.2mM/ (Lh) calculate, carry out three circulations.Under this reaction conditions, the degradation rate of aniline reaches more than 90%, and cycle index is low, and processing cost declines greatly.
Principle of the present invention is:
Amino benzene analog waste water enters electrolyzer, at low voltage 1 ~ 2V, under the condition of pH7 ~ 7.5, carry out electrolysis, in electrolytic process, add a certain amount of nitrite solution, aniline and nitrite generation diazonium salt react, remove amino, the carbon atom of former amino replacement place lacks an electronics, has extremely strong activity, very solution is connected on Graphite Electrodes, numerous aniline modified to electrode after, the specific surface area of electrode itself and electron transmission efficiency all obtain great raising, improve electrolytic efficiency with this.After low pressure self-assembly 2 ~ 5h, the more aniline of electrode surface self-assembly, now can stop adding nitrite and improve input voltage to 4 ~ 6V and carry out short period of time electrolysis, efficiently destroy degraded to the aniline of electrode surface modification.After high-pressure electrolysis 0.2 ~ 0.5h, again carry out low pressure modification, until aniline category matter concentration is lower than 10mg/L.
The present invention adopts high-low voltage interval to carry out, and low voltage is for promoting (no-voltage or high-voltage all modified-reaction can not occur) that react between nitrite and aniline, and high-voltage is for the material after degradation modification.
Compared with the method for existing electrolysis treatment aniline waste water, the present invention has following beneficial effect:
1) the present invention is directed to the aniline category matter in waste water, utilize phenyl amines self to be modified to electrode surface, improve electrode efficiency, accelerate the degraded of aniline simultaneously.
2) the present invention only adds Trace Nitrite in the reaction, clean low power consuming, simple to operate.
3) the electrode reusable edible in the present invention
Accompanying drawing explanation
Fig. 1 is the apparatus structure schematic diagram carrying out the inventive method.
Embodiment
Below in conjunction with accompanying drawing, the present invention is further illustrated.
Utilize a method for electrochemistry efficient degradation amino benzene analog waste water, this device can utilize the modified electrode of aniline own to improve electrochemical degradation efficiency; First carry out conventional short distance nitration to containing aniline waste water, the water outlet after short distance nitration is containing nitrite.Measure the concentration of short distance nitration water outlet nitrite.
Short distance nitration water outlet enters in electrolyzer 1, utilizes direct supply 3 first to carry out low voltage (1 ~ 2V) self-assembly 2 ~ 5h; Be (4 ~ 6V) electrolysis 0.2 ~ 0.5h carrying out high-voltage; Low voltage self-assembly and high-voltage electrolysis alternate cycles are carried out, and add short distance nitration water outlet after each loop ends in electrolyzer; The pH value controlling waste water in working cycle is 7 ~ 7.5.
Aniline and nitrite generation diazonium salt react antianode 1 and carry out modification, modified, under high pressure electrolysis, anode 1 surface material efficiently removed, and then low pressure modification-high pressure degraded, until aniline category matter is lower than 10mg/L, the spacing between electrolyzer inner anode and negative electrode is 2cm-10cm.
Embodiment 1
According to above-mentioned embodiment.The aniline category matter selected in embodiment is 2-fluoroaniline, 2-fluoroaniline starting point concentration is 100mg/L, anode adopts cylindrical graphite plate, negative electrode adopts graphite rod, and pH is 7, and low pressure is 2V, the self-assembly time is 3h, high pressure is 6V, electrolysis 0.2h, and first time circulation nitrite desired concn is 3mM/L; Circulate the beginning from second time, the short distance nitration water outlet at every turn added is by 1cm
2just to the nitrite amount needed for electrode area 1mM aniline be 0.2mM/ (Lh) calculate.After three circulations, 2-fluoroaniline clearance is 95%, TOC clearance is 91%, and defluorinate rate is 90%.
Embodiment 2
Embodiment is same as described above.The aniline category matter selected in embodiment is 2-fluoroaniline, 2-fluoroaniline starting point concentration is 100mg/L, anode adopts cylindrical graphite carbon felt, negative electrode adopts graphite rod, and pH is 7, and low pressure is 1V, electrolysis time is 5h, high pressure is 5V, electrolysis 0.5h, and first time circulation nitrite desired concn is 1mM/L; Circulate the beginning from second time, the short distance nitration water outlet at every turn added is by 1cm
2just to the nitrite amount needed for electrode area 1mM aniline be 0.02mM/ (Lh) calculate.After six circulations, 2-fluoroaniline clearance is 94%, TOC clearance is 90%, and defluorinate rate is 90%.
Embodiment 3
Embodiment is same as described above.The aniline category matter selected in embodiment is 2-fluoroaniline, 2-fluoroaniline starting point concentration is 100mg/L, anode adopts cylindrical graphite plate, negative electrode adopts graphite rod, and pH is 7, and low pressure is 1.5V, electrolysis time is 3h, high pressure is 5V, electrolysis 0.2h, and first time circulation nitrite desired concn is 2mM/L; Circulate the beginning from second time, the short distance nitration water outlet at every turn added is by 1cm
2just to the nitrite amount needed for electrode area 1mM aniline be 0.1mM/ (Lh) calculate.After five circulations, 2-fluoroaniline clearance is 97%, TOC clearance is 93%, and defluorinate rate is 94%.
Comparative example
Embodiment is same as described above.The aniline category matter selected in embodiment is 2-fluoroaniline, and 2-fluoroaniline starting point concentration is 100mg/L, and anode adopts cylindrical graphite plate, and negative electrode adopts graphite rod, and pH is 7, and low pressure is 2V, and electrolysis time is 3h, and high pressure is 6V, and electrolysis 0.2h, does not add nitrite.After three circulations, 2-fluoroaniline clearance is 55%, TOC clearance is 47%, and defluorinate rate is 50%.
Comparative example
Embodiment is same as described above.The aniline category matter selected in embodiment is 2-fluoroaniline, and 2-fluoroaniline starting point concentration is 100mg/L, and voltage control is at 6V, and after electrolysis 8h, 2-fluoroaniline clearance is 90%, TOC clearance is 81%, and defluorinate rate is 80%.
Claims (7)
1. utilize a method for pollutent self-assembly electro-chemical systems aniline degradation waste water, it is characterized in that, comprise the steps:
(1) aniline waste water is carried out short distance nitration, containing nitrite in the aniline waste water after short distance nitration; The aniline waste water carrying out short distance nitration is the waste water that specific conductivity is less than 1ms/cm;
(2) aniline waste water after short distance nitration is passed in electrolyzer, first carry out low voltage self-assembly; Carry out high-pressure electrolysis again; In this step, low voltage self-assembly and high-voltage electrolysis alternate cycles are carried out, in each circulation: low voltage is 1 ~ 2V, and the self-assembly time is 2 ~ 5h; High-voltage is 4 ~ 6V, and electrolysis time is 0.2 ~ 0.5h; In electrolyzer, the short distance nitration water outlet in step (1) is added, until Aniline concentration reaches required value after each loop ends.
2. utilize the method for pollutent self-assembly electro-chemical systems aniline degradation waste water according to claim 1, it is characterized in that, in working cycle, pH controls 7 ~ 7.5.
3. utilize the method for pollutent self-assembly electro-chemical systems aniline degradation waste water according to claim 1, it is characterized in that, step (2) circulation time of middle first time, waste water nitrite desired concn >1mM/L.
4. utilize the method for pollutent self-assembly electro-chemical systems aniline degradation waste water according to claim 1, it is characterized in that, circulate the beginning from second time, the short distance nitration water outlet at every turn added is by 1cm
2just to the nitrite amount needed for electrode area 1mM aniline be 0.02-0.2mM/ (Lh) calculate.
5. utilize the method for pollutent self-assembly electro-chemical systems aniline degradation waste water according to claim 1, it is characterized in that, the reaction electrode spacing in described electrolyzer is 2cm-10cm.
6. utilize the method for pollutent self-assembly electro-chemical systems aniline degradation waste water according to claim 1, it is characterized in that, the anode in described electrolyzer is one or several in graphite cake, graphite rod, carbon felt, carbon paper or graphite granule; Negative electrode in described electrolyzer is one or several in graphite cake, graphite rod, carbon felt, carbon paper or graphite granule.
7. utilize the method for pollutent self-assembly electro-chemical systems aniline degradation waste water according to claim 6, it is characterized in that, described anode is graphite anode, and negative electrode is graphite cathode, and graphite anode and graphite cathode area ratio are 5 ~ 100.
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| CN105600885B (en) * | 2015-11-11 | 2018-07-03 | 合肥工业大学 | It is a kind of to utilize the method for strengthening Inner sources Estrogen in absorption and low-voltage degradation collaboration removal water body |
| CN105948180B (en) * | 2016-06-06 | 2019-03-01 | 河海大学 | A kind of modified graphite electrode and the method for making anode electrochemical processing waste water from dyestuff |
| CN105948179A (en) * | 2016-06-06 | 2016-09-21 | 河海大学 | Preparation method and application of amino modified graphite electrode |
| CN113044931B (en) * | 2021-03-23 | 2023-01-20 | 南京环保产业创新中心有限公司 | Treatment device for nitroaromatic wastewater, and cathode preparation method and application thereof |
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