CN105668758A - Method for degrading organic wastewater by activating persulfates with in-situ sulfur-doped activated carbon - Google Patents

Method for degrading organic wastewater by activating persulfates with in-situ sulfur-doped activated carbon Download PDF

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CN105668758A
CN105668758A CN201610125208.5A CN201610125208A CN105668758A CN 105668758 A CN105668758 A CN 105668758A CN 201610125208 A CN201610125208 A CN 201610125208A CN 105668758 A CN105668758 A CN 105668758A
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active carbon
persulfate
organic
original position
waste water
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CN105668758B (en
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曾泽泉
郭耀萍
黄张根
杨洁扬
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Shanxi Institute of Coal Chemistry of CAS
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Shanxi Institute of Coal Chemistry of CAS
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    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/72—Treatment of water, waste water, or sewage by oxidation
    • C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation

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  • Chemical Kinetics & Catalysis (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Organic Chemistry (AREA)
  • Treatment Of Water By Oxidation Or Reduction (AREA)
  • Removal Of Specific Substances (AREA)

Abstract

The invention relates to a method for degrading organic wastewater by activating persulfates with in-situ sulfur-doped activated carbon. The method comprises the following steps: adding persulfates into an organic wastewater solution at normal temperature (the mole ratio of the persulfates to the organic pollutants is (1-50):1), regulating the pH value of the organic wastewater solution to 2-12 with 0.1 mol/L H2SO4 or 0.1 mol/L NaOH, adding in-situ sulfur-doped activated carbon, treating the wastewater solution for 1-3 hours, and carrying out solid-liquid separation, wherein the ratio of the in-situ sulfur-doped activated carbon to the organic wastewater solution is (0.1-0.3)g:1L. The method has the advantages of high organic pollutant removal efficiency and no secondary pollution.

Description

A kind of original position is mixed the method for sulphur active carbon activation persulfate degradation of organic waste water
Technical field
The invention belongs to a kind of processing method of degradation of organic waste water, a kind of method that is specifically related to original position and mixes sulphur active carbon activation persulfate degradation of organic waste water.
Background technology
In recent years, hydroxyl radical free radical high-level oxidation technology is widely used in organic wastewater with difficult degradation thereby processing because having the oxidisability feature that by force, selectively low, degradation efficiency is high. Due to its have advantages of easy and simple to handle, oxidisability is strong, Fenotn (H2O2/Fe2+) reagent oxidation technology becomes the high-level oxidation technology being most widely used. But this technology exists, applicable pH range is narrow, H2O2(oxidant) unstable, easily produce the problems such as mud. And stability is high, the persulfate of good water solubility has and H2O2Similar O – O key, sulfate radical free radical that can activated generation redox potential (2.5-3.1V) is higher, the pH scope of application is wider, thus efficiently remove persistent organic pollutants. Therefore, the persulfate high-level oxidation technology based on sulfate radical free radical, increasingly extensive in the application of field of wastewater in recent years.
Persulfate comprises peroxy-monosulfate and peroxydisulfate, it can be by thermal activation method, photoactivation method and transition metal ions activation method (CriticalReviewsinEnvironmentalScienceandTechnology, 45:1756 – 1800,2015) the sulfate radical free radical of generation strong oxidizing property, but these methods exist, and energy consumption is high, operating condition is harsh, system complex, secondary pollution problems, has limited the application of persulfate high-level oxidation technology in wastewater treatment.
If use a kind of nonmetal heterogeneous catalysis activation persulfate, so above shortcoming just can be overcome. And active carbon is because it has the advantages such as specific area is large, pore structure is flourishing, heat endurance is high, production cost is low, in field of heterogeneous catalysis, be used widely. In order to widen its scope of application, numerous scholars modify to improve its physicochemical characteristics and catalytic activity (RSCAdv., 2014,4,63110 – 63117 by means such as surface doping hetero atom, regulation and control pore structures to carbon material surface; AppliedCatalysisB:Environmental106 (2011) 390 – 397). Although it is strong, active high that surface doping hetero atom active carbon has advantages of catalytic capability, but the heteroatom functional that this method of modifying forms group is not to be embedded into equably in carbon skeleton, but be combined in its surface, therefore in use there will be stripping problem, even can make pore structure distortion, duct stop up, and then cause surface area to reduce, activity decreased. If direct carbonization contains heteroatomic presoma organic matter, so above shortcoming just can be overcome.
For overcoming the above problems, the present invention proposes the new method of utilizing original position to mix sulphur active carbon activation persulfate processing organic wastewater with difficult degradation thereby.
At present, there is no the application that invention relates to original position and mixes sulphur active carbon activation persulfate degradation of organic waste water.
Summary of the invention:
For solving problems of the prior art, the object of this invention is to provide a kind of organic pollutant removal efficiency high, the original position of non-secondary pollution is mixed the method for sulphur active carbon activation persulfate degradation of organic waste water.
For realizing above-mentioned technical purpose, original position of the present invention is mixed the method for sulphur active carbon activation persulfate degradation of organic waste water, comprises the steps:
Under normal temperature condition, in organic wastewater solution, add persulfate, making persulfate and organic pollution amount of substance ratio is 1-50:1, uses 0.1mol/LH2SO4Or 0.1mol/LNaOH to regulate the pH value of organic wastewater solution be 2-12, then add wherein original position and mix sulphur active carbon, to waste water solution processing 1h-3h, then carry out Separation of Solid and Liquid; Its situ is mixed sulphur active carbon: organic wastewater solution=0.1-0.3g:1L.
Persulfate as above is peroxy-monosulfate or peroxydisulfate.
It is to adopt roasting carbonization sulfur-bearing presoma and in this process, add chemical activating agent activation to make that original position as above is mixed sulphur active carbon, and its step of preparation process is:
Taking acetonitrile as a certain amount of 2 – thenyl alcohols of dissolution with solvents, slowly add and be dissolved with a certain amount of FeCl3Acetonitrile solution in, rapid stirring 15h at normal temperatures, successively with distilled water and acetone filter, washing for several times polythiophene sediment be colourless to filtrate, it is dry at 105 DEG C, obtain dry polythiophene. The polythiophene making is mixed according to the mass ratio of 1:2 with KOH, by it 600-800 DEG C of carbonization 1h under nitrogen atmosphere. HCl with 10% washs carbonized samples to remove residual inorganic matter, then it is dried under the condition of 110 DEG C to 24h after being neutrality with distilled water washing several to supernatant, obtains original position and mixes sulphur active carbon. Concrete preparation method is shown in document (MicroporousandMesoporousMaterials158 (2012) 318 – 323).
Compared with prior art, the present invention has following beneficial effect:
1. situ of the present invention is mixed sulphur active carbon except containing the oxygen-containing functional group such as carbonyl, quinonyl, also contain a large amount of thiophenic sulfurs and sulfuryl functional group, these groups can carry out oxidative degradation Organic Pollutants in Wastewater by high-efficiency continuous activation persulfate generation living radical as lewis base avtive spot.
2. the inventive method, compared with other catalyst, has not only improved the removal efficiency of catalytic efficiency and the organic pollution of catalyst, the secondary pollution problem of also having avoided the stripping of catalyst activity component to bring.
Brief description of the drawings:
Fig. 1 is the clearance variation diagram of embodiment 1 to hardly degraded organic substance;
Fig. 2 is the clearance variation diagram of embodiment 2 to hardly degraded organic substance.
Detailed description of the invention:
The present invention proposes a kind of original position and mix the method for sulphur active carbon activation persulfate degradation of organic waste water, be specially: under normal temperature condition, in waste water solution, add persulfate, making persulfate and organic pollution amount of substance ratio is 1:1-50:1, uses 0.1mol/LH2SO4Or 0.1mol/LNaOH to regulate the pH value of organic wastewater solution be 2-12, then to add wherein concentration be that the original position of 0.1-0.3g/L is mixed sulphur active carbon as catalyst, to water sample processing 1h-3h, then carries out Separation of Solid and Liquid.
The typical original position of preparing is mixed the method for sulphur active carbon and is:
3g2-thenyl alcohol is dissolved in 20ml acetonitrile solvent, slowly adds 100ml to be dissolved with 28.9gFeCl it3Acetonitrile solution in, rapid stirring 15h at normal temperatures, successively with distilled water and acetone filter, washing for several times polythiophene sediment be colourless to filtrate, it is dry at 105 DEG C, obtain dry polythiophene. Get three parts of dry polythiophenes, it is mixed according to the mass ratio of 1:2 with KOH respectively, with quartz ampoule roasting mixture under nitrogen atmosphere, temperature, with the speed of 3 DEG C/min, rises to respectively 600 DEG C, 700 DEG C, 800 DEG C by room temperature, and keeps temperature to continue calcining 1h, the original position that can obtain different temperatures roasting is mixed sulphur active carbon, count respectively ACS600, ACS700, ACS800.
Describe the present invention in detail below by specific embodiment.
The embodiment of the present invention is using phenol wastewater as typical organic wastewater with difficult degradation thereby. Phenol wastewater has the character of difficult for biological degradation, not only seriously destroys aquatic ecosystem and serious threat human health. Therefore in embodiment, select aldehydes matter as target contaminant.
Embodiment 1:
Get the pending water sample 200mL that contains coal chemical industrial waste water, wherein hardly degraded organic substance is parachlorophenol, and concentration is 80ppm. In this aqueous solution, add potassium peroxydisulfate, making potassium peroxydisulfate and parachlorophenol mol ratio is 24:1, add wherein again original position and mix sulphur active carbon (ACS800) 0.1g/L (wherein, the sintering temperature of ACS is 800 DEG C), water sample is processed to 130min, compared with independent persulfate oxidation method, clearance brings up to 100% by 2.82%.
Fig. 1 is that the present embodiment represents to adopt separately the clearance curve ， – △ – of persulfate oxidation degradation of organic waste water to represent the clearance curve of ACS800 activation persulfate catalyzing oxidizing degrading organic wastewater to the removal effect figure Tu Zhong – ○ – of parachlorophenol hardly degraded organic substance in coal chemical industrial waste water.
Embodiment 2:
Get the pending water sample 200mL that contains coal chemical industrial waste water, wherein hardly degraded organic substance is parachlorophenol, and concentration is 80ppm. In this aqueous solution, add potassium peroxydisulfate, making potassium peroxydisulfate and parachlorophenol mol ratio is 24:1, add wherein again original position and mix sulphur active carbon (ACS700) 0.1g/L (wherein, the sintering temperature of ACS is 700 DEG C), water sample is processed to 170min, compared with independent persulfate oxidation method, clearance brings up to 83.8% by 2.82%.
Fig. 2 is that the present embodiment represents to adopt separately the clearance curve ， – △ – of persulfate oxidation degradation of organic waste water to represent the clearance curve of ACS700 activation persulfate catalyzing oxidizing degrading organic wastewater to the removal effect figure Tu Zhong – ○ – of parachlorophenol hardly degraded organic substance in coal chemical industrial waste water.
Embodiment 3:
Get the pending water sample 200mL that contains coal chemical industrial waste water, wherein hardly degraded organic substance is parachlorophenol, and concentration is 80ppm. In this aqueous solution, add potassium peroxydisulfate, making potassium peroxydisulfate and parachlorophenol mol ratio is 24:1, add wherein again original position and mix sulphur active carbon (ACS600) 0.1g/L (wherein, the sintering temperature of ACS is 600 DEG C), water sample is processed to 170min, compared with independent persulfate oxidation method, clearance brings up to 52.3% by 2.82%.
Embodiment 4:
Get the pending water sample 200mL that contains pharmacy waste water, wherein hardly degraded organic substance is parachlorophenol, and concentration is 80ppm. In this aqueous solution, add a certain amount of potassium peroxydisulfate, making potassium peroxydisulfate and parachlorophenol mol ratio is 24:1, then adds wherein ACS8000.15g/L, and water sample is processed to 60min, compared with independent persulfate oxidation method, clearance brings up to 100% by 2.82%.
Embodiment 5:
Get the pending water sample 200mL that contains pharmacy waste water, wherein hardly degraded organic substance is parachlorophenol, and concentration is 80ppm. In this aqueous solution, add a certain amount of potassium peroxydisulfate, making potassium peroxydisulfate and parachlorophenol mol ratio is 3:1, then adds wherein ACS8000.1g/L, and water sample is processed to 170min, and compared with independent persulfate oxidation method, clearance brings up to 89% by 0.8%.
Embodiment 6:
Get the pending water sample 200mL that contains pharmacy waste water, wherein hardly degraded organic substance is parachlorophenol, and concentration is 80ppm. In this aqueous solution, add a certain amount of potassium peroxydisulfate, making potassium peroxydisulfate and parachlorophenol mol ratio is 50:1, then adds wherein ACS8000.1g/L, and water sample is processed to 125min, and compared with independent persulfate oxidation method, clearance brings up to 100% by 3.1%.
Embodiment 7:
Get the pending water sample 200mL that contains petroleum wastewater, wherein hardly degraded organic substance is parachlorophenol, and concentration is 80ppm. In this aqueous solution, add a certain amount of potassium peroxydisulfate, making potassium peroxydisulfate and parachlorophenol mol ratio is 24:1, uses 0.1mol/LH2SO4Regulating the pH value of waste water solution is 2.4, then adds wherein ACS8000.1g/L, and water sample is processed to 170min, and compared with independent persulfate oxidation method, clearance brings up to 93.8% by 2.3%.
Embodiment 8:
Get the pending water sample 200mL that contains petroleum wastewater, wherein hardly degraded organic substance is parachlorophenol, and concentration is 80ppm. In this aqueous solution, add a certain amount of potassium peroxydisulfate, making potassium peroxydisulfate and parachlorophenol mol ratio is 24:1, regulating the pH value of waste water solution with 0.1mol/LNaOH is 6.2, add wherein again ACS8000.1g/L, water sample is processed to 170min, compared with independent persulfate oxidation method, clearance brings up to 98.4% by 2.1%.
Embodiment 9:
Get the pending water sample 200mL that contains petroleum wastewater, wherein hardly degraded organic substance is parachlorophenol, and concentration is 80ppm. In this aqueous solution, add a certain amount of potassium peroxydisulfate, making potassium peroxydisulfate and parachlorophenol mol ratio is 24:1, regulating the pH value of waste water solution with 0.1mol/LNaOH is 8.4, add wherein again ACS8000.1g/L, water sample is processed to 170min, compared with independent persulfate oxidation method, clearance brings up to 95% by 2.72%.
Embodiment 10: get the pending water sample 200mL that contains paper pulp wastewater, wherein hardly degraded organic substance is parachlorophenol, and concentration is 80ppm. In this aqueous solution, add a certain amount of potassium peroxydisulfate, making potassium peroxydisulfate and parachlorophenol mol ratio is 24:1, regulating the pH value of waste water solution with 0.1mol/LNaOH is 10.7, add wherein again ACS8000.1g/L, water sample is processed to 170min, compared with independent persulfate oxidation method, clearance brings up to 82.6% by 3.08%.
Embodiment 11:
Get the pending water sample 200mL that contains waste water from dyestuff, wherein hardly degraded organic substance is phenol, and concentration is 80ppm. In this aqueous solution, add a certain amount of potassium peroxydisulfate, making potassium peroxydisulfate and phenol mol ratio is 24:1, then adds wherein ACS8000.1g/L, and water sample is processed to 150min, and compared with independent persulfate oxidation method, clearance brings up to 92.2% by 2.82%.

Claims (3)

1. original position is mixed a method for sulphur active carbon activation persulfate degradation of organic waste water, it is characterized in that comprising the steps:
Under normal temperature condition, in organic wastewater solution, add persulfate, making persulfate and organic pollution amount of substance ratio is 1-50:1, uses 0.1mol/LH2SO4Or 0.1mol/LNaOH to regulate the pH value of organic wastewater solution be 2-12, then add wherein original position and mix sulphur active carbon, to waste water solution processing 1h-3h, then carry out Separation of Solid and Liquid; Its situ is mixed sulphur active carbon: organic wastewater solution=0.1-0.3g:1L.
2. a kind of original position as claimed in claim 1 is mixed the method for sulphur active carbon activation persulfate degradation of organic waste water, it is characterized in that described persulfate is peroxy-monosulfate or peroxydisulfate.
3. a kind of original position as claimed in claim 1 is mixed the method for sulphur active carbon activation persulfate degradation of organic waste water, it is characterized in that comprising the steps:
Taking acetonitrile as a certain amount of 2 – thenyl alcohols of dissolution with solvents, slowly add and be dissolved with a certain amount of FeCl3Acetonitrile solution in, rapid stirring 15h at normal temperatures, successively with distilled water and acetone filter, washing for several times polythiophene sediment be colourless to filtrate, it is dry at 105 DEG C, obtain dry polythiophene; The polythiophene making is mixed according to the mass ratio of 1:2 with KOH, by it 600-800 DEG C of carbonization 1h under nitrogen atmosphere, HCl with 10% washs carbonized samples to remove residual inorganic matter, after supernatant is neutrality, it is dried under the condition of 110 DEG C to 24h for several times with distilled water washing again, obtains original position and mix sulphur active carbon.
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CN106391057A (en) * 2016-11-07 2017-02-15 中国科学院山西煤炭化学研究所 Preparation method and application of sulfur-doped activated carbon for degrading organic wastewater
CN108069488A (en) * 2016-11-17 2018-05-25 中国石油化工股份有限公司 A kind of acrylic fiber wastewater deep treatment method
CN108083416A (en) * 2017-12-21 2018-05-29 南昌航空大学 A kind of method that carbon material activation persulfate orientation is carbonylated and generates singlet oxygen
CN108503097A (en) * 2018-03-16 2018-09-07 昆明理工大学 A kind of processing method of organic pollution water
CN108996656A (en) * 2018-08-17 2018-12-14 河北工业大学 A kind of method that thermal activation sodium peroxydisulfate removes coal chemical industrial waste water COD with high salt
CN111875028A (en) * 2020-08-10 2020-11-03 导洁(北京)环境科技有限公司 Safe advanced oxidation method for refractory organics
CN112246265A (en) * 2020-09-04 2021-01-22 广东工业大学 Active complex for degrading bisphenol A and application thereof
CN113929202A (en) * 2021-11-25 2022-01-14 太原理工大学 Application of modified steel slag in activating persulfate to treat printing and dyeing wastewater
CN114573153A (en) * 2022-01-19 2022-06-03 中国科学院山西煤炭化学研究所 Method for degrading salt-containing organic wastewater by activating persulfate through electric field driving/pH regulation carbon electrode
CN114887435A (en) * 2022-05-05 2022-08-12 紫科装备股份有限公司 Process for treating waste water and gas in petroleum production

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CN106391057A (en) * 2016-11-07 2017-02-15 中国科学院山西煤炭化学研究所 Preparation method and application of sulfur-doped activated carbon for degrading organic wastewater
CN108069488A (en) * 2016-11-17 2018-05-25 中国石油化工股份有限公司 A kind of acrylic fiber wastewater deep treatment method
CN108083416B (en) * 2017-12-21 2020-12-01 南昌航空大学 Method for directionally generating singlet oxygen by activating persulfate through carbon carbonylation material
CN108083416A (en) * 2017-12-21 2018-05-29 南昌航空大学 A kind of method that carbon material activation persulfate orientation is carbonylated and generates singlet oxygen
CN108503097A (en) * 2018-03-16 2018-09-07 昆明理工大学 A kind of processing method of organic pollution water
CN108996656A (en) * 2018-08-17 2018-12-14 河北工业大学 A kind of method that thermal activation sodium peroxydisulfate removes coal chemical industrial waste water COD with high salt
CN111875028A (en) * 2020-08-10 2020-11-03 导洁(北京)环境科技有限公司 Safe advanced oxidation method for refractory organics
CN112246265A (en) * 2020-09-04 2021-01-22 广东工业大学 Active complex for degrading bisphenol A and application thereof
CN113929202A (en) * 2021-11-25 2022-01-14 太原理工大学 Application of modified steel slag in activating persulfate to treat printing and dyeing wastewater
CN114573153A (en) * 2022-01-19 2022-06-03 中国科学院山西煤炭化学研究所 Method for degrading salt-containing organic wastewater by activating persulfate through electric field driving/pH regulation carbon electrode
CN114573153B (en) * 2022-01-19 2023-12-19 中国科学院山西煤炭化学研究所 Method for degrading salt-containing organic wastewater by activating persulfate through carbon electrode under electric field driving/pH regulation
CN114887435A (en) * 2022-05-05 2022-08-12 紫科装备股份有限公司 Process for treating waste water and gas in petroleum production
CN114887435B (en) * 2022-05-05 2022-11-25 紫科装备股份有限公司 Process for treating waste water and gas in petroleum production

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