CN108892280A - A kind of processing method of the organic wastewater containing alkyl phenol - Google Patents
A kind of processing method of the organic wastewater containing alkyl phenol Download PDFInfo
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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
- C02F9/00—Multistage treatment of water, waste water or sewage
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
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- 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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- 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
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
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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
- C02F1/66—Treatment of water, waste water, or sewage by neutralisation; pH adjustment
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- 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
- C02F2001/007—Processes including a sedimentation step
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/34—Organic compounds containing oxygen
- C02F2101/345—Phenols
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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
- C02F2301/00—General aspects of water treatment
- C02F2301/08—Multistage treatments, e.g. repetition of the same process step under different conditions
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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
- C02F2303/00—Specific treatment goals
- C02F2303/04—Disinfection
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Abstract
A kind of processing method of the organic wastewater containing alkyl phenol, includes the following steps：（1）In deionized water by the dispersion of graphite oxide powder, using ultrasonic cleaning, aqueous solution of single-layer grapheme oxide is obtained；（2）Using lye by the pH value adjustment of aqueous solution of single-layer grapheme oxide to 9-11, hydrazine hydrate is then added and quickly stirs, obtains reproducibility graphene oxide；（3）Reproducibility graphene oxide is sufficiently mixed with thiocarbamide, tubular type kiln roasting is placed in, obtains N, S-rGO；（4）N, S-rGO and persulfate are added in the organic wastewater containing alkyl phenol, removes the alkyl phenol in organic wastewater.The reproducibility graphene oxide that the present invention passes through the nitrogen sulphur dual element doping of thermal decomposition method one-step synthesis, using the reproducibility graphene oxide of nitrogen sulphur dual element doping as catalyst, there is very strong catalysis excitation ability for persulfate, the potentiometric titrations of generation have very strong oxidative degradation ability to the organic wastewater containing alkyl phenol.
Description
Technical field
The present invention relates to a kind of processing method of organic wastewater, specially a kind of processing side of the organic wastewater containing alkyl phenol
Method.
Background technique
As industrial or agricultural and the level of urbanization rapidly develop, using induced by alkyl hydroxybenzene as the steroid incretion interferent of representative
Also it inevitably imports into environment water.Existing numerous studies discovery, even if horizontal in very low exposure concentrations, induced by alkyl hydroxybenzene
Pollutant still has endocrine disruption toxicity to human body and animal and plant body.Currently, the processing method for phenol wastewater mainly has
Extraction, absorption method, chemical oxidization method, biochemical treatment process etc..Extraction energy consumption is high, and extractant easily occurs and remains on subsequent waste water
In, influence subsequent treatment process；Absorption method is easy to operate, is suitable for the lower waste water of amount containing phenol, but equipment one-time investment
It is larger, and adsorbent reactivation is difficult.Rising in recent years based on Fenton（Fenton）The high-level oxidation technology of reaction（AOP）Most
To be universal, it is to utilize ferrous ion（Fe2+）Chain reaction catalysis between hydrogen peroxide generates free radical, has relatively strong
Oxidability, oxidizing potential is only second to fluorine, and Fenton reagent can be especially suitable without most of organic matters in selective oxidation water
The oxidation processes of the organic wastewater hard to work for bio-refractory or general chemical oxidation.However, the technology is in addition in water
Introduced outside H2O2 and Fe2+ in body, act on the hydroxyl radical free radical generated selectivity is not high and oxygen to certain hard-degraded substances
It is bad to change efficiency.
The shortcomings that in order to overcome traditional Fenton method, is based on potentiometric titrations（SO42-•）High-level oxidation technology meet the tendency of
And it gives birth to.Persulfate advanced oxidation processes are to make persulfuric acid by means such as heating, transition metal ion catalyst, ultraviolet lights
Radical ion（S2O82-）Generate potentiometric titrations（SO42-•）.Potentiometric titrations are electrophilic free radical, when organic matter
Contain amino in structure（-NH2）, hydroxyl（-OH）, carboxyl（-COOH）And alkoxy（-OR）When equal electron-donating groups, sulfate radical
Easily with the type organic redox reaction occurs for free radical, by organic matter degradation be the small molecular organic acid of nonhazardous, H2O and
CO2 etc..However advanced oxidation processes have the defects that it is different degrees of, such as to equipment requirement harshness, degradation effect is poor, and subsequent processing is numerous
It is miscellaneous, therefore catalytic oxidation comes into being.Since the toxicity characteristic of metallics limits its application in practical water process,
Nonmetalloid（N, S, B）The graphene oxide composite material of load progresses into the visual field of people as catalyst, and multielement is mixed
Miscellaneous reproducibility graphene has catalytic performance more better than single element doping reproducibility graphene.
Currently, the graphene oxide main method of synthetic non-metallic element load is hydro-thermal, solvent heat etc., this synthesis process
With process complexity, the disadvantages of time-consuming, it is therefore desirable to develop it is a kind of prepare it is simple, the high nonmetalloid load of success rate
The preparation method of graphene oxide.
Summary of the invention
The purpose of the present invention is to provide a kind of processing methods of organic wastewater containing alkyl phenol, solve asking in background technique
Topic.
A kind of processing method of the organic wastewater containing alkyl phenol, includes the following steps：
（1）After organic wastewater containing alkyl phenol is collected, into coagulating basin, coagulant is added, removes the major part in sewage
COD, coloration；
（2）Organic wastewater after coagulating treatment enters sedimentation basin, settles 10-20h, removes the large particulate matter in waste water；
（3）Organic wastewater after settlement treatment enters oxidation pond, and N, S-rGO and persulfate is added, and mixes post-processing 1-2h,
Remove the alkyl phenol in organic wastewater；
（4）Organic wastewater after oxidation-treated enters settling tank, adjusts PH to 7-8,2-3h is settled, after processing water outlet is sterilized
Qualified discharge；
（5）By used N, S-rGO is recovered by filtration, and is recycled after drying.
Further, the mass ratio of alkyl phenol is 1 in the N, S-rGO and organic wastewater:2000-3000.
Further, the persulfate is K2S2O8, and K2S2O8 and N is added, and the mass ratio of S-rGO is 1:1.
The preparation method of a kind of N, S-rGO composite material, which is characterized in that include the following steps：
（1）In deionized water by the dispersion of graphite oxide powder, it using supersonic wave cleaning machine ultrasound 30-60min, obtains mono-layer oxidized
Graphene aqueous solution；
（2）Using lye by the pH value adjustment of aqueous solution of single-layer grapheme oxide to 9-11, hydrazine hydrate is then added and quickly stirs
5-10min, then 95 DEG C of stirring in water bath 4-8, centrifugation, washing, vacuum drying obtain reproducibility graphene oxide；
（3）Reproducibility graphene oxide is sufficiently mixed with thiocarbamide, tubular type kiln roasting 1-3h is placed in, obtains N, S-rGO.
Further, the lye is ammonium hydroxide.
Further, the constitution of the hydrazine hydrate and graphene oxide ratio is 9-12mL:1g.
Further, the mass ratio of the thiocarbamide and graphene oxide is 2-5:1.
Further, the tube furnace is quartz tube furnace, 5-10 DEG C of heating rate/min, maturing temperature 300-500
℃。
By transmission electron microscope, Raman and electrochemical method to the pattern of material doped front and back, structure and electrocatalysis characteristic into
Characterization is gone, the results show that many defects occurs in the reproducibility surface of graphene oxide structure after doping, with Raman characterization knot
Fruit is consistent, it was demonstrated that the doping of nitrogen element sulphur destroys the original silk shape flat configuration of graphene oxide.Electrochemical Characterization method is into one
Step proves that material has stronger electronics transfer and capacitive property after doping.In short, material catalytic degradation performance obtains after doping
Large increase.
Beneficial effect：
1, reproducibility graphene oxide of the present invention by the nitrogen sulphur dual element doping of thermal decomposition method one-step synthesis, short flow,
Success rate is high.
, the present invention using the reproducibility graphene oxide of nitrogen sulphur dual element doping as catalyst, for persulfate tool
There is very strong catalysis excitation ability, the potentiometric titrations of generation have very strong oxidative degradation to the organic wastewater containing alkyl phenol
Ability.
Detailed description of the invention
Fig. 1 is the transmission electron microscope that 1 synthetic material of embodiment adulterates front and back morphology characterization（TEM）Figure.
Fig. 2 is the material doped front and back Raman characterization figure of embodiment 2.
Fig. 3 is the electrochemical Characterization figure of the material doped front and back cyclic voltammetric of embodiment 3.
Fig. 4 is the electrochemical Characterization figure of the material doped front and back electrochemical impedance of embodiment 3.
Fig. 5 is 4 closed matereial cycle performance inquiry experiment figure of embodiment.
Fig. 6 is thiocarbamide content to nitrogen sulfur doping reproducibility graphene oxide catalytic degradation performance influence diagram.
Specific embodiment
In order to be easy to understand the technical means, the creative features, the aims and the efficiencies achieved by the present invention, tie below
Specific embodiment is closed, the present invention is further explained.Wherein embodiment 1-3 mainly illustrates that material is catalyzed after thiocarbamide dosage adulterates it
The influence of performance.Embodiment 4 mainly illustrates material repeat performance after doping.
Embodiment 1：
1. taking 150 mg graphite oxide powder（GOs）It is scattered in the beaker equipped with 300 mL deionized waters, uses ultrasonic cleaning
40 min of machine ultrasound（180 W）, until solution can't see apparent particle.
2. the above pH value of solution is adjusted to 10 using ammonium hydroxide, 10 mL hydrazine hydrates are added（N2H4•H2O）After be vigorously stirred rather
Clock continues to stir 5 h under 95 DEG C of water bath conditions, by final product centrifugation, washing, vacuum drying.
3. 1 g of reproducibility graphene oxide and 1 g thiocarbamide that take above step to obtain are transferred to porcelain boat after being sufficiently mixed,
Argon atmosphere quartz tube type kiln roasting 1 h, 10 DEG C/min of heating rate, 350 DEG C of maturing temperature, the product that will be obtained（N,S-
rGO-1）It is fully ground broken, uses ethyl alcohol and milli-Q water, 60 DEG C of dryings of vacuum.
4. the degradation experiment that initial concentration is the alkyl phenol of 20 μ g/L carries out in 250-mL band plug conical flask, in 298 K
Under the conditions of temperature, it is 200 rpm that setting water bath with thermostatic control, which shakes rate, the N of preparation is added, S-rGO makes its concentration in the solution
50 mg/L, are eventually adding 50 mg potassium peroxydisulfates, and catalysis degeneration experiment starts.
5. respectively 0,1,5,10,20,30,60 min of time take out 10 mL, using after Extraction with n-Octanol use liquid phase color
It composes mass spectrum tandem mass spectrum and measures object residual concentration Ct.
It is found as shown in Figure 1, being characterized by TEM, more defect occurs in graphene oxide accordion flat surface after doping
Gap, it can be seen that the doping of nitrogen element sulphur destroys graphene oxide script structure.
Embodiment 2：
1. taking 150 mg graphite oxide powder（GOs）It is scattered in the beaker equipped with 300 mL deionized waters, uses ultrasonic cleaning
40 min of machine ultrasound（180 W）, until solution can't see apparent particle.
2. the above pH value of solution is adjusted to 10 using ammonium hydroxide, 10 mL hydrazine hydrates are added（N2H4•H2O）After be vigorously stirred rather
Clock continues to stir 5 h under 95 DEG C of water bath conditions, by final product centrifugation, washing, vacuum drying.
3. 1 g of reproducibility graphene oxide and 2 g thiocarbamides that take above step to obtain are transferred to porcelain boat after being sufficiently mixed,
Argon atmosphere quartz tube type kiln roasting 1 h, 10 DEG C/min of heating rate, 350 DEG C of maturing temperature, the product that will be obtained（N,S-
rGO-2）It is fully ground broken, uses ethyl alcohol and milli-Q water, 60 DEG C of dryings of vacuum.
4. the degradation experiment that initial concentration is the alkyl phenol of 20 μ g/L carries out in 250-mL band plug conical flask, in 298 K
Under the conditions of temperature, it is 200 rpm that setting water bath with thermostatic control, which shakes rate, the N of preparation is added, S-rGO makes its concentration in the solution
50 mg/L, are eventually adding 50 mg potassium peroxydisulfates, and catalysis degeneration experiment starts.
5. respectively 0,1,5,10,20,30,60 min of time take out 10 mL, using after Extraction with n-Octanol use liquid phase color
It composes mass spectrum tandem mass spectrum and measures object residual concentration Ct.
As shown in Fig. 2, the peak intensity ratio ID/IG value at the peak graphene oxide D and the peak G is 1.18 before adulterating, ID/IG after doping
Value becomes 1.37, and material degree of graphitization is lower after illustrating doping, and many defects occurs in surface texture, as a result with TEM result
Unanimously.
Embodiment 3：
1. taking 150 mg graphite oxide powder（GOs）It is scattered in the beaker equipped with 300 mL deionized waters, uses ultrasonic cleaning
40 min of machine ultrasound（180 W）, until solution can't see apparent particle.
2. the above pH value of solution is adjusted to 10 using ammonium hydroxide, 10 mL hydrazine hydrates are added（N2H4•H2O）After be vigorously stirred rather
Clock continues to stir 5 h under 95 DEG C of water bath conditions, by final product centrifugation, washing, vacuum drying.
3. 1 g of reproducibility graphene oxide for taking above step to obtain and 3 g of thiocarbamide are transferred to porcelain boat after being sufficiently mixed,
Argon atmosphere quartz tube type kiln roasting 1 h, 10 DEG C/min of heating rate, 350 DEG C of maturing temperature, the product that will be obtained（N,S-
rGO-3）It is fully ground broken.Use ethyl alcohol and milli-Q water, 60 DEG C of dryings of vacuum.
4. the degradation experiment that initial concentration is the alkyl phenol of 20 μ g/L carries out in 250-mL band plug conical flask, in 298 K
Under the conditions of temperature, it is 200 rpm that setting water bath with thermostatic control, which shakes rate, the N of preparation is added, S-rGO makes its concentration in the solution
50 mg/L, are eventually adding 50 mg potassium peroxydisulfates, and catalysis degeneration experiment starts.
5. respectively 0,1,5,10,20,30,60 min of time take out 10 mL, using after Extraction with n-Octanol use liquid phase color
It composes mass spectrum tandem mass spectrum and measures object residual concentration Ct.
As shown in Figure 3 and Figure 4, under the conditions of O2 atmosphere, 0.1 M KOH solution, adulterate before GO oxidation-reduction potential be-
The oxidation-reduction potential of 0.344 V, N after doping, S-rGO are that -0.334 V is increased, corresponding 0.17 mA of peak current
Cm-2 is also greater than 0.12 mA cm-2 of graphene oxide, its catalytic performance improves a lot after illustrating graphene oxide doped.
The capacitive property of reproducibility graphene oxide is more excellent after adulterating it can be seen from electrochemical impedance result.
Embodiment 4：
1. used material is recovered by filtration by bottle,suction and is placed on 60 DEG C of vacuum oven drying for use.
2. the degradation experiment that initial concentration is the alkyl phenol of 20 μ g/L carries out in 250-mL band plug conical flask, in 298 K
Under the conditions of temperature, it is 200 rpm that setting water bath with thermostatic control, which shakes rate, and the N that recycling obtains is added, and S-rGO keeps it dense in the solution
Degree is 50 mg/L, is eventually adding 50 mg potassium peroxydisulfates, and catalysis degeneration experiment starts.
3. respectively 0,1,5,10,20,30,60 min of time take out 10 mL, using after Extraction with n-Octanol use liquid phase color
It composes mass spectrum tandem mass spectrum and measures object residual concentration Ct.
4. after recycling the material 3 times, catalysis persulfate so that degrade target contaminant ability almost without
Any decrease, it was demonstrated that this kind of material has good reusing, and it is entirely titanium dioxide that it, which can degrade target contaminant,
Carbon and water meet green energy resource requirement.
As shown in figure 5, obtain N by reclaiming by filtration, after S-rGO, by it under vacuum condition dry, same steps weight
It is found after using 3 times again, catalytic degradation performance still keeps good.
As shown in fig. 6, the nitrogen sulfur content for being carried on surface of graphene oxide is also increased as thiocarbamide content increases
Add, therefore, the efficiency of the material catalytic degradation target contaminant is improved as nitrogen sulfur content increases, and illustrates higher nitrogen
Element sulphur doping content is more advantageous to its catalytic degradation.
Basic principles and main features and advantages of the present invention of the invention have been shown and described above, the present invention is not by upper
The limitation of embodiment is stated, the above embodiments and description only illustrate the principle of the present invention, is not departing from the present invention
Under the premise of spirit and scope, various changes and improvements may be made to the invention, these changes and improvements both fall within claimed
In the scope of the invention, the scope of the present invention is defined by the appended claims and its equivalents.
Claims (8)
1. a kind of processing method of organic wastewater containing alkyl phenol, which is characterized in that include the following steps：
After organic wastewater containing alkyl phenol is collected, into coagulating basin, coagulant is added, remove most COD in sewage,
Coloration；
Organic wastewater after coagulating treatment enters sedimentation basin, settles 10-20h, removes the large particulate matter in waste water；
Organic wastewater after settlement treatment enters oxidation pond, and N, S-rGO and persulfate is added, and mixes post-processing 1-2h, goes
Except the alkyl phenol in organic wastewater；
Organic wastewater after oxidation-treated enters settling tank, adjusts PH to 7-8, settles 2-3h, reaches after processing water outlet is sterilized
Mark discharge；
By used N, S-rGO is recovered by filtration, and is recycled after drying.
2. the processing method of the organic wastewater according to claim 1 containing alkyl phenol, which is characterized in that the N, S-rGO and
The mass ratio of alkyl phenol is 1 in organic wastewater:2000-3000.
3. the processing method of the organic wastewater according to claim 1 containing alkyl phenol, which is characterized in that the persulfate is
K2S2O8, K is added2S2O8And the mass ratio of N, S-rGO are 1:1.
4. a kind of processing method of organic wastewater containing alkyl phenol according to claim 1, which is characterized in that the N, S-
The preparation method of rGO includes the following steps：
In deionized water by the dispersion of graphite oxide powder, using supersonic wave cleaning machine ultrasound 30-60min, mono-layer oxidized stone is obtained
Black aqueous solution；
Using lye by the pH value adjustment of aqueous solution of single-layer grapheme oxide to 9-11, hydrazine hydrate is then added and quickly stirs 5-
10min, then 95 DEG C of stirring in water bath 4-8, centrifugation, washing, vacuum drying obtain reproducibility graphene oxide；
Reproducibility graphene oxide is sufficiently mixed with thiocarbamide, tubular type kiln roasting 1-3h is placed in, obtains N, S-rGO.
5. the preparation method of N according to claim 4, S-rGO composite material, which is characterized in that the lye is ammonium hydroxide.
6. the preparation method of N according to claim 4, S-rGO composite material, which is characterized in that the hydrazine hydrate and oxygen
The constitution ratio of graphite alkene is 9-12mL:1g.
7. the preparation method of N according to claim 4, S-rGO composite material, which is characterized in that the thiocarbamide and oxidation
The mass ratio of graphene is 1-3:1.
8. the preparation method of N according to claim 4, S-rGO composite material, which is characterized in that the tube furnace is stone
English tube furnace, 5-10 DEG C of heating rate/min, maturing temperature are 300-500 DEG C.
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| CN114486407A (en) * | 2020-10-26 | 2022-05-13 | 中国石油化工股份有限公司 | Oxidant for sample graphitization pretreatment and preparation method and application thereof |
| CN114772700A (en) * | 2022-04-24 | 2022-07-22 | 湖南大学 | Method for removing sulfadimidine by using ferro-manganese bimetallic organic framework/modified reduced graphene oxide composite material |
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| CN110237818A (en) * | 2019-06-14 | 2019-09-17 | 上海工程技术大学 | A kind of preparation method and application of nitrogen sulphur codope charcoal |
| CN114486407A (en) * | 2020-10-26 | 2022-05-13 | 中国石油化工股份有限公司 | Oxidant for sample graphitization pretreatment and preparation method and application thereof |
| CN113371704A (en) * | 2021-01-27 | 2021-09-10 | 青岛烯碳瑞尔新材料科技有限公司 | Green and simple preparation method of high-conductivity and high-dispersity graphene |
| CN114772700A (en) * | 2022-04-24 | 2022-07-22 | 湖南大学 | Method for removing sulfadimidine by using ferro-manganese bimetallic organic framework/modified reduced graphene oxide composite material |
| CN114772700B (en) * | 2022-04-24 | 2024-05-17 | 湖南大学 | Method for removing sulfadimidine by utilizing ferro-manganese bimetal organic framework/modified reduced graphene oxide composite material |
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