CN109534481A - A kind of processing method of phenol wastewater - Google Patents
A kind of processing method of phenol wastewater Download PDFInfo
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- CN109534481A CN109534481A CN201811542565.7A CN201811542565A CN109534481A CN 109534481 A CN109534481 A CN 109534481A CN 201811542565 A CN201811542565 A CN 201811542565A CN 109534481 A CN109534481 A CN 109534481A
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- Prior art keywords
- phenol wastewater
- processing method
- added
- pani
- phenol
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Classifications
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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
- C02F1/722—Oxidation by peroxides
-
- 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
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/26—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24
- B01J31/28—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24 of the platinum group metals, iron group metals or copper
-
- 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
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
- C02F1/302—Treatment of water, waste water, or sewage by irradiation with microwaves
-
- 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
-
- C—CHEMISTRY; METALLURGY
- 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
Abstract
The invention discloses a kind of processing methods of phenol wastewater, comprising the following steps: H is added in phenol wastewater2O2、Fe3O4/ PANI composite material, then carries out microwave treatment.A kind of processing method of phenol wastewater proposed by the present invention, phenolic substances has many advantages, such as that the reaction time is short, treatment effeciency is high, easy to operate, easily controllable, without secondary pollution in this method degrading waste water.
Description
Technical field
The present invention relates to technical field of waste water processing more particularly to a kind of processing methods of phenol wastewater.
Background technique
Phenol pollution in environment refers mainly to pollution of the phenolic compound to water body, and phenol wastewater is endangered in the world today
Greatly, wide one of the industrial wastewater of pollution range is the important sources of water pollution in environment.Many industrial circles such as coal gas,
Coking, oil refining, metallurgy, machine-building, glass, petrochemical industry, lumber fibre, chemical organic synthesis industry, plastics, medicine, agriculture
Contain phenol in the waste water of the industry discharge such as medicine, paint.Phenolic compound belongs to the very strong organic pollutant of toxicity, most of nitre
Base phenol has mutagenic effect;The methyl-derivatives of phenol not only teratogenesis, and it is carcinogenic.Their toxicity is with replacing journey on aromatic ring
The increase of degree and increase.If these waste water can pollute big gas and water, soil and food without processing, direct emission, irrigated farmland
Product.
It is very strong to generate oxidability because reaction condition is mild, equipment is simple, low in cost, high-efficient for Fenton method
It is useless to be widely used in handling papermaking, printing and dyeing, coking almost without selectively oxidative degradation organic matter for hydroxyl radical free radical (OH)
In the toxic organic wastewater difficult to degrade such as water.But there are catalyst to be difficult to recycle and reuse, is also easy to produce iron for homogeneous Fenton method
Mud, H2O2The features such as utilization rate is low constrains its practical application in water process.Therefore, conventional homogeneous Fenton method need to be added
To improve.
Magnetic Nano Fe3O4Because it has the characteristics that good superparamagnetism, thermal stability, high reaction activity, easily prepared, no
The advantages of only remaining homogeneous Fenton reaction, can excite H2O2Generate OH, and be easy to Magneto separate recycling, iron from
Subflow is lost less, obtains extensive concern in type Fenton catalyst research.But nanometer Fe3O4There are mutual between magnetic dipole for particle
Effect is easy to reunite, causes catalytic activity to reduce, influence H2O2The effect of degrading phenol substance.
Summary of the invention
Technical problems based on background technology, the invention proposes a kind of processing method of phenol wastewater, this method
Phenolic substances has that the reaction time is short, treatment effeciency is high, easy to operate, easily controllable, without secondary pollution etc. excellent in degrading waste water
Point.
The processing method of a kind of phenol wastewater proposed by the present invention, comprising the following steps: H is added in phenol wastewater2O2、
Fe3O4/ PANI composite material, then carries out microwave treatment.
Preferably, phenol wastewater, H2O2、Fe3O4Weight ratio between/PANI composite material is 40-60:0.15-0.3:
40-60;Wherein, H2O2Concentration be 25-35wt%.
Preferably, microwave power 70-210W, microwave treatment time 4-6min.
Preferably, Fe3O4/ PANI composite material is prepared by following technique:
S1, by nanometer Fe3O4It mixes, is ultrasonically treated with ethanol water, lauryl sodium sulfate and aniline is then added,
Concentrated hydrochloric acid is added after mixing, stirs, obtains material A;
S2, ammonium persulfate aqueous solution is added in material A, stirs, is filtered, clean, dry, grinding obtains Fe3O4/
PANI composite material.
Preferably, Fe3O4In/PANI composite material preparation process, nanometer Fe3O4, ethanol water, dodecyl sulphate
Sodium, aniline, concentrated hydrochloric acid, the weight ratio between ammonium persulfate aqueous solution are 0.02-0.03:100-120:0.01-0.02:0.4-
0.6:5-7:9-11;Wherein, the volumetric concentration of ethanol water is 8-12%, and the concentration of concentrated hydrochloric acid is 35-40wt%, persulfuric acid
The concentration of aqueous ammonium is 6-8wt%.
Preferably, in S1, ultrasonic power 30-50kHz, sonication treatment time 15-20min.
Preferably, in S1,30-40min is stirred at room temperature.
Preferably, in S2,12-13h is stirred at room temperature.
Preferably, in S2, water and ethanol washing are specially successively used in cleaning, until filtrate is clarified.
Preferably, in S2, drying temperature is 65-70 DEG C, drying time 15-17h.
Fe in the present invention3O4/ PANI composite material is in its preparation process, first by nanometer Fe3O4It is used in ethanol water
Ultrasonic power ultrasound a period of time of 30-50kHz, not only make Fe3O4It is uniformly dispersed in system solution, also effectively enhancing
Fe3O4Activity shortens subsequent mixing time, improves nanometer Fe3O4With the composite effect of PANI, obtained Fe3O4/ PANI composite wood
Expect that it has both nanometer Fe3O4With the performance of both PANI, effectively solution nanometer Fe3O4It the phenomenon that reuniting in the solution avoids influencing
Subsequent phenolic substances degradation effect, and Fe2+It is not easy to dissolve out, not will cause secondary pollution, while compared to simple nanometer
Fe3O4, with more adsorption site, the phenolic substances in aqueous solution can be fixed, be conducive to whole system reaction into
Row, more preferably to the removal effect of phenolic substances, while Fe3O4/ PANI composite material has good environmental stability and wave absorbtion
Can, Fe is improved under microwave treatment3O4The catalytic activity of/PANI composite material, further excites H2O2Generate OH, enhancing
H2O2The effect of system degrading phenol substance.Then microwave treatment is used, one side microwave improves system local temperature, cooperation
Fe3O4/ PANI composite material, effectively facilitates H2O2It decomposes and generates OH, contaminant molecule polarization is accelerated to realize and oxidant
(H2O2) synergistic effect, significantly increase H of the present invention2O2Phenolic substances in system degrading waste water;The office that another aspect microwave generates
Portion's high temperature can also generate certain pyrolysis to the phenolic substances in water.A kind of processing of phenol wastewater proposed by the present invention
Method, in this method degrading waste water phenolic substances have the reaction time is short, treatment effeciency is high, it is easy to operate, easily controllable, without two
The advantages that secondary pollution.
Specific embodiment
In the following, technical solution of the present invention is described in detail by specific embodiment.
Embodiment 1
The processing method of a kind of phenol wastewater proposed by the present invention, comprising the following steps: H is added in phenol wastewater2O2、
Fe3O4/ PANI composite material, then carries out microwave treatment.
Wherein, Fe3O4/ PANI composite material is prepared by following technique:
S1, by nanometer Fe3O4It mixes, is ultrasonically treated with ethanol water, lauryl sodium sulfate and aniline is then added,
Concentrated hydrochloric acid is added after mixing, stirs, obtains material A;
S2, ammonium persulfate aqueous solution is added in material A, stirs, is filtered, clean, dry, grinding obtains Fe3O4/
PANI composite material.
Embodiment 2
The processing method of a kind of phenol wastewater proposed by the present invention, comprising the following steps: useless containing phenol at 40 parts by weight
The H that 0.15 part of concentration is 25wt% is added in water2O2, 40 parts of Fe3O4/ PANI composite material, then carries out microwave treatment, wherein
Microwave power is 70W, microwave treatment time 6min.
Wherein, Fe3O4/ PANI composite material is prepared by following technique:
S1, by weight by 0.02 part of nanometer Fe3O4The ethanol water for being 8% with 100 parts of volumetric concentrations mixes, ultrasound
20min is handled, 0.01 part of lauryl sodium sulfate and 0.4 part of aniline is then added, 5 parts of concentration are added after mixing is
The concentrated hydrochloric acid of 35wt%, is stirred at room temperature 40min, obtains material A;
S2, the ammonium persulfate aqueous solution that 9 parts of concentration are 6wt% is added in material A, 13h is stirred at room temperature, pass through
Filter, then water and ethanol washing are successively used, until filtrate is clarified, then in 65 DEG C of dry 17h, grinding obtains Fe3O4/ PANI is compound
Material.
Embodiment 3
The processing method of a kind of phenol wastewater proposed by the present invention, comprising the following steps: useless containing phenol at 60 parts by weight
The H that 0.3 part of concentration is 35wt% is added in water2O2, 60 parts of Fe3O4/ PANI composite material, then carries out microwave treatment, wherein
Microwave power is 210W, microwave treatment time 4min.
Wherein, Fe3O4/ PANI composite material is prepared by following technique:
S1, by weight by 0.03 part of nanometer Fe3O4The ethanol water for being 12% with 120 parts of volumetric concentrations mixes, ultrasound
15min is handled, 0.02 part of lauryl sodium sulfate and 0.6 part of aniline is then added, 7 parts of concentration are added after mixing is
The concentrated hydrochloric acid of 40wt%, is stirred at room temperature 30min, obtains material A;
S2, the ammonium persulfate aqueous solution that 11 parts of concentration are 8wt% is added in material A, 12h is stirred at room temperature, pass through
Filter, then water and ethanol washing are successively used, until filtrate is clarified, then in 70 DEG C of dry 15h, grinding obtains Fe3O4/ PANI is compound
Material.
Embodiment 4
The processing method of a kind of phenol wastewater proposed by the present invention, comprising the following steps: useless containing phenol at 50 parts by weight
The H that 0.2 part of concentration is 30wt% is added in water2O2, 50 parts of Fe3O4/ PANI composite material, then carries out microwave treatment, wherein
Microwave power is 150W, microwave treatment time 5min.
Wherein, phenol wastewater chooses bisphenol-A (BPA) aqueous solution of 10mg/L.
Fe3O4/ PANI composite material is prepared by following technique:
S1, by weight by 0.025 part of nanometer Fe3O4The ethanol water for being 10% with 100 parts of volumetric concentrations mixes, and surpasses
Then 0.01 part of lauryl sodium sulfate and 0.5 part of aniline is added in sonication 18min, 6 parts of concentration are added after mixing and are
The concentrated hydrochloric acid of 37wt%, is stirred at room temperature 35min, obtains material A;
S2, the ammonium persulfate aqueous solution that 10.76 parts of concentration are 7wt% is added in material A, 12.5h is stirred at room temperature,
It is filtered, then successively uses water and ethanol washing, until filtrate is clarified, then in 68 DEG C of dry 16h, grinding obtains Fe3O4/PANI
Composite material.
Embodiment 5
The processing method of a kind of phenol wastewater proposed by the present invention, comprising the following steps: useless containing phenol at 55 parts by weight
The H that 0.28 part of concentration is 30wt% is added in water2O2, 55 parts of Fe3O4/ PANI composite material, then carries out microwave treatment, wherein
Microwave power is 180W, microwave treatment time 5.5min.
Wherein, Fe3O4/ PANI composite material is prepared by following technique:
S1, by weight by 0.028 part of nanometer Fe3O4The ethanol water for being 11.5% with 115 parts of volumetric concentrations mixes,
It is ultrasonically treated 16min, 0.018 part of lauryl sodium sulfate and 0.55 part of aniline is then added, 6.5 parts of addition is dense after mixing
Degree is the concentrated hydrochloric acid of 36wt%, and 38min is stirred at room temperature, obtains material A;
S2, the ammonium persulfate aqueous solution that 10.5 parts of concentration are 6.5wt% is added in material A, is stirred at room temperature
12.5h is filtered, then successively uses water and ethanol washing, until filtrate is clarified, then in 68 DEG C of dry 15.5h, grinding is obtained
Fe3O4/ PANI composite material.
Comparative example
With in embodiment 4 the difference is that, by Fe3O4/ PANI composite material is substituted for nanometer Fe3O4。
Experimental analysis:
The phenol wastewater handled in embodiment 4 and comparative example is passed through 0.22 μm of filter within the set time to filter to take
Sample, using the concentration of BPA in phenol wastewater after high performance liquid chromatography detection processing, wherein chromatography column condition:
AgilentEclipsePlusC18 column (100mm × 2.1mm, 3.5 μm);Mobile phase: methanol-ultrapure water (80: 20, V/V);Stream
Speed: 1.0mL/min;Column temperature: 35 DEG C;Wavelength 270nm.The eliminating rate of absorption of BPA in phenol wastewater is calculated, discovery uses embodiment
4 with comparative example in processing method be respectively 82.1% and 56.3% to the removal rate of BPA.The experimental results showed that using Fe3O4/
PANI composite material is compared to nanometer Fe3O4Has the effect of better degrading phenol substance.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Anyone skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (10)
1. a kind of processing method of phenol wastewater, which comprises the following steps: H is added in phenol wastewater2O2、
Fe3O4/ PANI composite material, then carries out microwave treatment.
2. the processing method of phenol wastewater according to claim 1, which is characterized in that phenol wastewater, H2O2、Fe3O4/ PANI is multiple
Weight ratio between condensation material is 40-60:0.15-0.3:40-60;Wherein, H2O2Concentration be 25-35wt%.
3. the processing method of phenol wastewater according to claim 1 or claim 2, which is characterized in that microwave power 70-210W, it is micro-
Wave handles the time as 4-6min.
4. the processing method of phenol wastewater described in any one of -3 according to claim 1, which is characterized in that Fe3O4/ PANI is compound
Material is prepared by following technique:
S1, by nanometer Fe3O4It mixes, is ultrasonically treated with ethanol water, lauryl sodium sulfate and aniline, mixing is then added
Concentrated hydrochloric acid is added after uniformly, stirring obtains material A;
S2, ammonium persulfate aqueous solution is added in material A, stirs, is filtered, clean, dry, grinding obtains Fe3O4/ PANI is multiple
Condensation material.
5. the processing method of phenol wastewater described in any one of -4 according to claim 1, which is characterized in that Fe3O4/ PANI is compound
In material preparation process, nanometer Fe3O4, ethanol water, lauryl sodium sulfate, aniline, concentrated hydrochloric acid, ammonium persulfate aqueous solution
Between weight ratio be 0.02-0.03:100-120:0.01-0.02:0.4-0.6:5-7:9-11;Wherein, ethanol water
Volumetric concentration is 8-12%, and the concentration of concentrated hydrochloric acid is 35-40wt%, and the concentration of ammonium persulfate aqueous solution is 6-8wt%.
6. the processing method of phenol wastewater described in any one of -5 according to claim 1, which is characterized in that in S1, ultrasonic power
For 30-50kHz, sonication treatment time 15-20min.
7. the processing method of phenol wastewater described in any one of -6 according to claim 1, which is characterized in that in S1, at room temperature
Stir 30-40min.
8. the processing method of phenol wastewater described in any one of -7 according to claim 1, which is characterized in that in S2, at room temperature
Stir 12-13h.
9. the processing method of phenol wastewater described in any one of -8 according to claim 1, which is characterized in that in S2, cleaning is specific
Successively to use water and ethanol washing, until filtrate is clarified.
10. the processing method of phenol wastewater described in any one of -9 according to claim 1, which is characterized in that in S2, drying temperature
It is 65-70 DEG C, drying time 15-17h.
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Citations (4)
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---|---|---|---|---|
CN1149586C (en) * | 1997-10-31 | 2004-05-12 | 美商纳克公司 | Electromagnetic shielding |
CN104971778A (en) * | 2015-06-30 | 2015-10-14 | 天津大学 | Preparation method and applications of ferriferrous oxide-polyaniline-gold nano composite material |
CN105771934A (en) * | 2016-05-06 | 2016-07-20 | 扬州大学 | Preparation method of nanometer magnetic adsorbent with core-shell structure |
CN106242136A (en) * | 2016-08-31 | 2016-12-21 | 浙江奇彩环境科技股份有限公司 | A kind of processing method containing pyridines waste water |
-
2018
- 2018-12-17 CN CN201811542565.7A patent/CN109534481A/en active Pending
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1149586C (en) * | 1997-10-31 | 2004-05-12 | 美商纳克公司 | Electromagnetic shielding |
CN104971778A (en) * | 2015-06-30 | 2015-10-14 | 天津大学 | Preparation method and applications of ferriferrous oxide-polyaniline-gold nano composite material |
CN105771934A (en) * | 2016-05-06 | 2016-07-20 | 扬州大学 | Preparation method of nanometer magnetic adsorbent with core-shell structure |
CN106242136A (en) * | 2016-08-31 | 2016-12-21 | 浙江奇彩环境科技股份有限公司 | A kind of processing method containing pyridines waste water |
Non-Patent Citations (4)
Title |
---|
严梅等: "纳米Fe3O4 负载聚苯胺对染料的协同催化降解", 《中国环境科学》 * |
张宝营: "微波辅助Fe3O4/H2O2类Fenton法处理罗丹明B废水", 《山东化工》 * |
王迎军: "《新型材料科学与技术 无机材料卷 上》", 31 October 2016, 华南理工大学出版社 * |
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Application publication date: 20190329 |