CN108059229A - A kind of method of iron carbon activation persulfate processing high-concentration hardly-degradable alkaline waste liquor - Google Patents

A kind of method of iron carbon activation persulfate processing high-concentration hardly-degradable alkaline waste liquor Download PDF

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Publication number
CN108059229A
CN108059229A CN201711389800.7A CN201711389800A CN108059229A CN 108059229 A CN108059229 A CN 108059229A CN 201711389800 A CN201711389800 A CN 201711389800A CN 108059229 A CN108059229 A CN 108059229A
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China
Prior art keywords
zero
persulfate
alkaline waste
waste liquor
iron
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CN201711389800.7A
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Chinese (zh)
Inventor
陈家斌
黄天寅
王骁
赵雪瑞
史祯琦
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Suzhou University of Science and Technology
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Suzhou University of Science and Technology
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Priority to CN201711389800.7A priority Critical patent/CN108059229A/en
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    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/72Treatment of water, waste water, or sewage by oxidation
    • C02F1/725Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/28Treatment of water, waste water, or sewage by sorption
    • C02F1/281Treatment of water, waste water, or sewage by sorption using inorganic sorbents
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/10Inorganic compounds
    • C02F2101/101Sulfur compounds

Abstract

The present invention relates to a kind of methods of iron carbon activation persulfate processing high-concentration hardly-degradable alkaline waste liquor:At normal temperatures and pressures into the alkaline waste liquor containing high-concentration hardly-degradable organic matter, a certain amount of Zero-valent Iron (Fe is added in0) and activated carbon (AC) and persulfate (PS), it stirs evenly, reacts 2~3h in the case where initial pH is alkaline condition, you can oxidative degradation pollutant.The present invention cooperates with active oxidation agent by adding Zero-valent Iron and activated carbon into alkaline waste liquor, generates sulfate radical, hydroxyl radical free radical oxidation stain substance, so as to degrading alkaline waste liquid;Compared with traditional Fenton oxidation technology, there is the broader pH scope of applications, save acid adding neutralization procedure, not only contribute to the removal of pollutant, and reduce financial cost.In addition, utilize Fe0With AC as catalyst, activation PS is made to generate SO4 Efficiency significantly improve, be more advantageous to the efficient process of alkaline waste liquor.

Description

A kind of method of iron carbon activation persulfate processing high-concentration hardly-degradable alkaline waste liquor
Technical field
The present invention relates to field of waste liquid treatment, and in particular to a kind of to utilize the difficult drop of iron carbon activation persulfate removal high concentration The method for solving organic pollution in alkaline waste liquor.
Background technology
Industrial wastes typically refers to the dangerous material with environment hidden danger.Often pollutant concentration is high for industrial wastes, water quality into Divide complexity, biodegradability poor, be the important content of field of water pollution control.Common industrial wastes processing mode mainly has biology Treatment technology, materializing strategy technology and advanced oxidation treatment technology, biologic treating technique generally requires pollutant concentration low, highly concentrated It is low to spend treatment effeciency, especially alkaline industrial wastes, biodegradability is extremely low, need to usually be located in advance into biological processing unit Reason, Traditional materialized technical finesse efficiency is low, and the scope of application is small, and with respect to above two treatment technology, chemical oxidation is in process cycle Upper shorter, cost is relatively low, small to the destruction of environment, and for being generally difficult to handle organic chemical contaminant oxidation with higher Imitate stable treatment effect.Based on the limitation of alkaline waste liquor chemical removal techniques, advanced oxidation (Advanced Oxidation Processes) technology receives more and more attention on removal alkaline waste liquor.
High-level oxidation technology, feature are that largely the hydroxyls with Strong oxdiative ability are oxidant for generation, and in high temperature height It is small molecule the organic pollutant degradation of macromolecular under the reaction conditions such as pressure, the irradiation of electricity, sound, light, catalyst.It is wherein fragrant The oxidation technology that pauses is most common traditional high-level oxidation technology, however its pH scope of application is small (i.e. acid), and processing cost is high, iron The problems such as mud yield is big limits its extensive use.In recent years, the high-level oxidation technology based on potentiometric titrations increasingly by To the attention of people, since it is to the efficient removal rate of persistent organic pollutants and highly selective, have developed into difficult The new technology of degradation of organic waste water.The general potentiometric titrations that high activity is generated using activation persulfate, oxidative degradation water Toxic organic pollutant in body promotes most of hardly degraded organic substance oxidative degradations.
Big compared with the outside energy needed for photocatalytic method, the complexity of thermocatalytic method heating system utilizes transition metal Ion makees catalyst, and the effect of degradation of contaminant is fine, but part metals ion can cause environment secondary pollution, while gold Belong to ion (Fe2+) and persulfate reaction generation SO4 -Although efficiency it is very fast, reduce SO instead4 -Utilization rate, Catalyst service life is short, and utilization rate is relatively low, and processing cost is high, and the time is long, is unfavorable for the lasting, efficient and fast of COD in waste water Speed removal.In summary, how easier, efficient processing high-concentration hardly-degradable alkaline waste liquor has become the art urgent need It solves the problems, such as.
The content of the invention
The purpose of the present invention provides a kind of utilization iron carbon activation persulfate aiming at above-mentioned deficiency of the prior art The method for handling high-concentration hardly-degradable alkaline waste liquor.Specifically, give up at normal temperatures and pressures to the alkalescence containing hardly degraded organic substance In liquid, a certain amount of Zero-valent Iron (Fe is added in0) and activated carbon (AC) and persulfate (PS), in the case where pH is the primary condition of alkalescence React 2~3h, you can oxidative degradation pollutant.
The present invention generates sulfate radical, hydroxyl certainly by adding Zero-valent Iron and activated carbon active oxidation agent into alkaline waste liquor By base oxidation stain substance, so as to degrading alkaline waste liquid.Since iron carbon activation PS generates SO in alkaline conditions4 -Have higher Oxidation-reduction potential, and compared with traditional Fenton oxidation technology, there is the broader pH scope of applications, save in acid adding and walk Suddenly, the removal of pollutant is not only contributed to, and reduces financial cost.The present invention utilizes Fe0With AC as catalyst, make work Change PS and generate SO4 -Efficiency significantly improve, action time is short, is more advantageous to the efficient process of alkaline waste liquor, wherein reactant Be it is easy to operate, save acid adding neutralize, solid PS be readily transported, so as to provide a kind of new high-level oxidation technology in alkalescence Application in industrial wastes processing.
To achieve these goals, iron carbon activation persulfate processing high-concentration hardly-degradable is utilized the present invention provides a kind of The method of alkaline waste liquor, includes the following steps:
(1) Zero-valent Iron, activated carbon and persulfate are added into high-concentration hardly-degradable alkaline waste liquor;
(2) stir evenly, initial pH is alkaline condition;
(3) 2~3h is reacted at room temperature, you can oxidation removal polluter.
Since industry enterprise of Suzhou City quantity is more, the dangerous material yield such as waste liquid is larger, and environment hidden danger is fairly common.Industry enterprise Industry after the liquid waste processing of generation for that can not meet regulatory requirements, at present often by the unified collection of waste liquid, centralized processing.The present invention The high-concentration hardly-degradable alkaline waste liquor, for high-concentration hardly-degradable alkalescence industrial wastes after dilution, initial COD value is 10160~10690mg/L.
The mass ratio of Zero-valent Iron and activated carbon is 2: 1~6: 1, preferably 3: 1~5: 1 in above-mentioned steps (1), is most preferably 4: 1 or so.
Zero-valent Iron and activated carbon are as dual catalyst in above-mentioned steps (1), and persulfate is as oxidant.
In above-mentioned steps (1) dosage of Zero-valent Iron be 2.6~6.6g/L, optimum dosage 4.7g/L, activated carbon Dosage is 1.1~1.3g/L, optimum dosage 1.2g/L.
Persulfate is 20~28g/L it is preferable to use sodium peroxydisulfate, dosage in above-mentioned steps (1), and optimum dosage is 22g/L, i.e. 0.092mol/L.
Above-mentioned dosage refers both to calculate what is obtained on the basis of the volume of high-concentration hardly-degradable alkaline waste liquor.
The rotating speed of stirring is 200r/min in above-mentioned steps (2), and pH value is 10~11.
In technical solution provided by the invention, preferably iron is zeroth order micron iron, and activated carbon is less than 100 mesh powders for grain size Activated carbon.
In technical solution provided by the invention, the effect of iron carbon activation persulfate in alkaline conditions, is carried out without acid adding It neutralizes.
In addition, technical scheme selects Zero-valent Iron and activated carbon, as dual catalyst, persulfate is as oxidation Agent degrades to high-concentration hardly-degradable alkaline waste liquor, can obtain good removal effect.
The present invention includes following advantageous effect:
1st, technical solution provided by the present invention uses Zero-valent Iron and activated carbon as dual catalyst.Zero-valent Iron can conduct Fe2+Generating source substitute Fe2+Persulfate is activated, slowly discharges Dissolvable Fe2+, avoid excessive Fe2+It is free with sulfate radical Base forms competition, so as to improve activation efficiency, reaches better degradation effect.Activated carbon is both good adsorbent and urges Agent, surface oxygen functional group play key player in catalytic process.There is significant synergistic effect in the two so that this Invention generates the effect better than the prior art.
2nd, using persulfate as oxidant, persulfuric acid salts substances high water solubility, such as sodium peroxydisulfate, solubility can in water Up to 73g/100g (25 DEG C), for the hydrogen peroxide of liquid, the persulfate of solid is more convenient for transporting in practical engineering application It is defeated and commercially available cheap thus of low cost, workable in practical engineering application.
3rd, for method provided by the invention under high alkalinity condition (pH is 10~11), the activation of iron carbon generates SO4-, hydrogen-oxygen Radical ion can also activate persulfate and generate living radical, more efficient degradation pollutant, also be produced during simultaneous reactions Raw hydrogen ion, reduces system pH, is more advantageous to subsequently being further processed.Using persulfate advanced oxidation technology, in alkali Property under the conditions of realize high-concentration hardly-degradable waste liquid efficient process be discovered in recent years new technology, for traditional advanced oxidation skill Art (Fenton oxidation technology) is often suitable for sour environment, and alkaline condition effect is poor;High alkalinity environment is unfavorable for microorganism Growth, before biological treatment often by waste liquid acid adding and, drug consumption is big, the high technical barrier of financial cost, should Method can not only save in acid adding and link, reduces financial cost;It can also further be produced after persulfate degradation of contaminant Raw hydrogen ion, reduces system pH, is more advantageous to subsequently being further processed.Therefore, technical scheme overcomes traditional sweet smell The problem that applicable pH range is small, iron cement yield is big, while save acid adding neutralization procedure, reduces processing financial cost, have compared with Good economic benefit.
4th, invention also provides a kind of persulfate high-level oxidation technologies in the application of water treatment field, solve difficulty The processing problem of degrading alkaline waste liquid has expanded the scope of application of persulfate technology significantly, promotes persulfate emerging technology Promotion and application in terms of waste water (liquid) processing.
Description of the drawings
Fig. 1 is in 200r/min, and same concentrations persulfate adds the COD degradation graph under the conditions of different catalysts.
Fig. 2 is in 200r/min, same concentrations persulfate and micron Zero-valent Iron, adds various concentration activated carbon (C) item COD degradation graph under part.
Fig. 3 is in 200r/min, same concentrations persulfate and the proportion of Zero-valent Iron and activated carbon (Fe/C)=4: 1 condition Under, the COD degradation graph of different Fe and C dosages.
Fig. 4 is the COD drops under the conditions of 200r/min, various concentration persulfate, same concentrations Zero-valent Iron and activated carbon Solution curve figure.
Specific embodiment
Below by several embodiments specific embodiment that the present invention will be described in detail, but not to the claim of the present invention Do any restriction.
It is collected in following each embodiments using unification, is organic by diluting the high concentration of the COD >=10000mg/L handled Industrial wastewater is as processing sample.
Embodiment 1
Sodium peroxydisulfate solid (2.2g) is taken to add in the high-concentration organic industrial waste water of the 100ml of pH=10.5, is added respectively Enter 1. micron Zero-valent Iron (i.e. the Zero-valent Iron of micron level) 0.47g, 2. C powder 0.12g, 3. micron Zero-valent Iron 0.47g and C powder 0.12g.Being placed in water bath chader, oscillating reactions 3h, i.e. completion utilize persulfate solution to height under room temperature in 200r/min The removal of COD in concentration organic industrial sewage.As shown in Figure 1:In the case where only adding in C powder, drops of the COD in waste water in 3h Solution rate is 76.2%;In the case where only adding in micron zeroth order iron powder, degradation rates of the COD in waste water in 3h levels off to 70.7%;In the case of adding in C powder and micron Zero-valent Iron, degradation rates of the COD in waste water in 3h is more than 86.4%, is said well Understand that activity powdered carbon and Zero-valent Iron can play significant its synergistic activation effect during persulfate degrades COD.
Embodiment 2
By 2.2g sodium peroxydisulfates, 0.47g microns of Zero-valent Irons take the C powder of 0.06g, 0.09g, 0.12g and 0.16g to add respectively In the high-concentration organic industrial waste water for entering the 100ml of pH=10.5, it is placed in water bath chader and is shaken under room temperature in 200r/min Reaction 3h is swung, that is, completes to utilize the micron Zero-valent Iron of persulfate solution and different specific weight and active removal of the powdered carbon to COD.Such as Shown in Fig. 2, the removal rate of COD respectively reaches 59.25%, 61.6%, 86.4%, 60.8% in this example, illustrates to work as Zero-valent Iron Best results when proportion with activated carbon is about 4: 1.
Embodiment 3
By 2.2g sodium peroxydisulfates, 0.24g microns of Zero-valent Irons and 0.06g carbon dusts, 0.35g micron Zero-valent Iron and 0.09g carbon are taken Powder, 0.47g micron Zero-valent Iron and 0.12g carbon dusts, 0.94g micron Zero-valent Iron and 0.24g carbon dusts, 1.88g micron Zero-valent Iron and 0.47g carbon dusts in the high-concentration organic industrial waste water for the 100ml for being added separately to pH=10.5, are placed in water bath chader and exist Concussion reaction 3h, i.e. completion utilize different microns under the conditions of persulfate solution and identical iron-carbon ratio to 200r/min under room temperature The removal of Zero-valent Iron and carbon dust dosage to COD.As shown in figure 3, in this example the removal rate of COD respectively reach 57.5%, 65.5%th, 86.4%, 74.4%, 76.2%, the optimum dosage for illustrating Zero-valent Iron and carbon dust is respectively 4.7g/L and 1.2g/L.
Embodiment 4
0.47g microns of Zero-valent Irons and 0.12g activated carbon are taken, takes the sodium peroxydisulfate of 1.2g, 1.7g, 2.2g and 3.0g, respectively It is added in the high-concentration organic industrial waste water of the 100ml of pH=10.5, is placed in water bath chader in 200r/min room temperature conditions Lower concussion reaction 3h completes to utilize removal of the various concentration persulfate solution to COD.As shown in figure 4, COD in this example Removal rate respectively reach 73.0%, 75.8%, 86.4%, 79.0%, illustrate when sodium peroxydisulfate dosage be 22g/L when effect Most preferably.
In conclusion the present invention, using persulfate as oxidant, is based on using carbon dust and micron Zero-valent Iron as catalyst Micron Zero-valent Iron catalysis persulfate generates the principle of potentiometric titrations, and micron Zero-valent Iron activation PS (persulfate) is generated SO4 -, there is higher oxidation-reduction potential, and partly decline with longer compared with the hydroxyl radical free radical in Fenton oxidation method Phase;Hydrogen ion is also generated during simultaneous reactions.This method can not only save in acid adding and link, reduces financial cost;It crosses Hydrogen ion can also be further generated after sulfate degradation of contaminant, system pH is reduced, is more advantageous to subsequently being further processed; It can carry out under room temperature, reaction condition is mild;It is easy to get in addition, sulfate and Zero-valent Iron are relatively inexpensive in life, zeroth order Iron is harmless, secondary pollution will not be caused to environment, while persulfate, micron Zero-valent Iron are solid particle, are convenient for Transport has more practicability and operability for the processing of a large amount of actual waste waters, and process costs are low, in high concentration organic industry Waste water COD is degraded and removal aspect has broad application prospects.
Embodiment provided above is the better embodiment of the present invention, only is used for facilitating illustrating the present invention, not to this hair The limitation of bright work in any form, any those of ordinary skill in the art, if putting forward skill not departing from the present invention In the range of art feature, using the equivalent embodiment locally changed or modified made by disclosed technology contents, and Without departing from the technical feature content of the present invention, in the range of still falling within the technology of the present invention feature.

Claims (10)

  1. A kind of 1. method of iron carbon activation persulfate processing high-concentration hardly-degradable alkaline waste liquor, which is characterized in that the method Comprise the following steps:
    (1) Zero-valent Iron, activated carbon and persulfate are added into high-concentration hardly-degradable alkaline waste liquor;
    (2) stir evenly, initial pH is alkaline condition;
    (3) 2~3h is reacted at room temperature, you can oxidation removal polluter.
  2. 2. according to the method described in claim 1, it is characterized in that, at the beginning of the step (1) middle and high concentration difficult degradation alkaline waste liquor Beginning COD value is 10160~10690mg/L.
  3. 3. according to the method described in claim 1, it is characterized in that, the mass ratio of the Zero-valent Iron and activated carbon is 2: 1~6: 1。
  4. 4. according to the method described in claim 3, it is characterized in that, the mass ratio of the Zero-valent Iron and activated carbon is about 4: 1.
  5. 5. according to the method described in claim 1, it is characterized in that, Zero-valent Iron and activated carbon are urged as double in the step (1) Agent, for persulfate as oxidant, the persulfate is sodium peroxydisulfate.
  6. 6. according to the method described in claim 5, it is characterized in that, in the step (1) dosage of Zero-valent Iron for 2.6~ 6.6g/L, the dosage of activated carbon is 1.1~1.3g/L.
  7. 7. according to the method described in claim 1, it is characterized in that, in the step (1) dosage of persulfate for 20~ 28g/L。
  8. 8. according to the method described in claim 1, it is characterized in that, the rotating speed of stirring is 200r/min, pH in the step (2) It is worth for 10~11.
  9. 9. according to the method described in claim 1, it is characterized in that, the iron is zeroth order micron iron.
  10. 10. according to the method described in claim 1, it is characterized in that, the activated carbon is less than 100 mesh powders activity for grain size Charcoal.
CN201711389800.7A 2017-12-20 2017-12-20 A kind of method of iron carbon activation persulfate processing high-concentration hardly-degradable alkaline waste liquor Pending CN108059229A (en)

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CN108609716A (en) * 2018-05-24 2018-10-02 上海亚新建设工程有限公司 A kind of method of the slow-release persulfate degradating chloro hydrocarbon of iron-charcoal optimization
CN108996752A (en) * 2018-08-10 2018-12-14 金华市升阳资源再利用有限公司 A method of recycling low concentration nickel from the raffinate waste water of nickel
CN109721138A (en) * 2019-03-05 2019-05-07 北京林业大学 A kind of method of electric field-enhanced over cure acid group free radical processing dyeing waste water
CN109851026A (en) * 2019-01-08 2019-06-07 同济大学 A kind of dye waste water treatment method
CN110479753A (en) * 2019-07-30 2019-11-22 广东工业大学 A kind of microwave catalysis oxidation device and method of organic polluted soil

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CN104891719A (en) * 2015-05-11 2015-09-09 东华大学 Method for pre-treating organic industrial wastewater based on ferric-carbon micro-electrolysis activated persulfate
CN107055738A (en) * 2017-01-19 2017-08-18 浙江大学 A kind of method that Zero-valent Iron activation persulfate removes Taste and odor compounds in water removal

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CN103435144A (en) * 2013-08-27 2013-12-11 华南理工大学 Method for utilizing heterogeneous catalyst to efficiently activate persulfate so as to treat organic wastewater
CN103896388A (en) * 2014-03-26 2014-07-02 华南理工大学 Method for treating organic wastewater by using double catalysts to heterogeneously activate persulfates
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CN108609716A (en) * 2018-05-24 2018-10-02 上海亚新建设工程有限公司 A kind of method of the slow-release persulfate degradating chloro hydrocarbon of iron-charcoal optimization
CN108996752A (en) * 2018-08-10 2018-12-14 金华市升阳资源再利用有限公司 A method of recycling low concentration nickel from the raffinate waste water of nickel
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CN109851026A (en) * 2019-01-08 2019-06-07 同济大学 A kind of dye waste water treatment method
CN109721138A (en) * 2019-03-05 2019-05-07 北京林业大学 A kind of method of electric field-enhanced over cure acid group free radical processing dyeing waste water
CN110479753A (en) * 2019-07-30 2019-11-22 广东工业大学 A kind of microwave catalysis oxidation device and method of organic polluted soil

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