CN106582875B - It is catalyzed the active carbon based composite catalyst and preparation method thereof of persulfate degradation of dye methyl orange - Google Patents
It is catalyzed the active carbon based composite catalyst and preparation method thereof of persulfate degradation of dye methyl orange Download PDFInfo
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- CN106582875B CN106582875B CN201611214048.8A CN201611214048A CN106582875B CN 106582875 B CN106582875 B CN 106582875B CN 201611214048 A CN201611214048 A CN 201611214048A CN 106582875 B CN106582875 B CN 106582875B
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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
- 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
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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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- 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
- C02F2101/308—Dyes; Colorants; Fluorescent agents
Abstract
The present invention relates to a kind of active carbon based composite catalysts for being catalyzed persulfate degradation of dye methyl orange, it is characterized in that, specific steps include: first to load to cobaltosic oxide on graphite oxide, it is again that the graphite oxide of supported cobaltosic oxide and oxycellulose is compound, then by compound with active carbon is compound prepares active carbon based composite catalyst, Potassium Monopersulfate (PMS) finally is added into the water containing methyl orange, pH value is adjusted, active carbon based composite catalyst is added and degrades at a certain temperature.Catalyst of the invention can be used at normal temperature, it is applied widely, this heterogeneous cobaltosic oxide/graphite oxide/oxycellulose/active carbon/PMS catalyzing oxidizing degrading system has high catalytic efficiency, the advantages that oxidability is strong, and reusability is good, particularly pertinent is that Catalyst Adsorption ability is strong, mechanical strength is big, it can be deposited to waste water bottom after the reaction was completed, convenient for recycling, can be applied to the fields such as sewage treatment and environmental improvement.
Description
Technical field
The present invention relates to a kind of composite materials applied in the fields such as sewage treatment and environmental improvement, more particularly to one kind
It is catalyzed the active carbon based composite catalyst and preparation method thereof of persulfate degradation of dye methyl orange.
Background technique
Active carbon has flourishing microcellular structure and special surface property, but separately as adsorbent absorption pollutant
It is not able to satisfy the requirement of development of modern industry.The pore structure for adjusting active carbon, is modified surface group, such as urging
The carrier of the metal ion of change effect, can be improved its property and specific absorption and catalytic performance is processed in stain disease
The effect of journey.Li Weifeng etc. with the catalyst of the preparations such as activated carbon supported Cu, Fe, Ni, Mn to the oxidation of actual dying at
Reason all has certain catalytic capability (Li Weifeng, Zhu Shemin, Song Tianshun, Chen Yingwen, Shen Shubao Metal Supported activated carbon catalysis
Oxidation processes dyeing waste water [J] Nanjing University of Technology journal 2006.7,5-8).The prosperous equal Study On The Activated Carbons area load Ag of remaining plan+、Ni2+、Cu2+Or Zn2+Ion, can be improved activated carbon adsorption benzothiophene sulfide ability (remaining plan is prosperous, Li Zhong, Xia Qibin,
Xi Hongxia activated carbon surface loaded metal ion adsorbs influence [J] the Journal of Chemical Industry and Engineering 2006.8.1943- of benzothiophene to it
1948)。
PMS also known as potassium peroxymonosulfate, can transition metal, heating or it is ultraviolet in the case where generate SO4-·
(Beitz T., Bechmann W., Mitzner R.Investigations of reactions of selected
azaarenes with redicals in Water.1.Hydroxyl and sulfate
Radicals.J.Phys.Chem.A., 1998,102 (34): 6760-6765) and be widely used in environmental treatment.
Summary of the invention
The problem to be solved by the invention is to provide a kind of active carbon base for being catalyzed persulfate degradation of dye methyl orange is multiple
Close catalyst, this catalyst compared with typical catalyst, be less susceptible to decompositions, excellent adsorption, recycling reuse it is active it is higher,
It recycles more convenient.
To solve the above-mentioned problems, the present invention provides a kind of active carbon bases for being catalyzed persulfate degradation of dye methyl orange
The preparation method of composite catalyst, which is characterized in that first load to cobaltosic oxide on graphite oxide, then will four oxidation of load
The graphite oxide of three cobalts and oxycellulose are compound, then by compound with active carbon is compound prepares active carbon based composite catalysis
Finally Potassium Monopersulfate (PMS) is added into the water containing methyl orange in agent, adjusts pH value, and active carbon based composite catalysis is added
Agent is degraded.
Preferably, the active carbon based composite catalyst the preparation method comprises the following steps:
Step 1: graphite oxide powder is added in n-hexyl alcohol, just evenly dispersed suspension is formed it by ultrasound
Cabaltous nitrate hexahydrate is separately dissolved in another n-hexyl alcohol by liquid, formed after red solution with the suspension containing graphite oxide
Liquid is mixed, and being stirred at room temperature mixes two kinds of substances uniformly, is then heated at reflux mixture at 140 DEG C
Reaction system is cooled to room temperature after reaction by 12h, centrifuge washing, and washed repeatedly with ethyl alcohol with remove n-hexyl alcohol and its
In sundries, finally the product of acquisition is dried for standby in 60 DEG C of vacuum drying oven；
Step 2: high-speed stirred dissolves oxycellulose to sodium hydroxide/thiocarbamide/urea liquid at low temperature, obtain transparent
Oxycellulose solution, product is then removed into insoluble matter and bubble by high speed centrifugation, by cobaltosic oxide/graphite oxide
Composite powder ultrasonic disperse 1h, is uniformly mixed with cellulose solution, and mixed liquor is mixed with active carbon again, final to be uniformly mixed
Slurries filtered using polytetrafluoroethylene film, with hydrochloric acid pH is adjusted to neutrality before filtering, dry 12h at 60 DEG C in air, i.e.,
Obtain active carbon based composite catalyst.
Preferably, the additional amount of the Potassium Monopersulfate is 0.4-10mmol/L.
Preferably, the additional amount of the active carbon based composite catalyst is 0.8-1.6g/L.
Preferably, the pH value is 4-10.
Preferably, the temperature of the degradation is 15-60 DEG C；Degradation time is 2-14min.
Preferably, the initial concentration of the methyl orange is 0.1-1mmol/L.
Preferably, the additional amount of the Potassium Monopersulfate is 2mmol/L；The additional amount of active carbon based composite catalyst
For 1.2g/L；PH value is 7；Degradation temperature is 25 DEG C, degradation time 8min；The initial concentration of methyl orange is 0.2m in water
mol/L.Under the combination of the treatment conditions, there is better treatment effeciency, the removal rate of methyl orange is 99.5% or more.
It urges the present invention also provides a kind of active carbon base using above-mentioned catalysis persulfate degradation of dye methyl orange is compound
The active carbon based composite catalyst of the catalysis persulfate degradation of dye methyl orange of the preparation method preparation of agent.
Preferably, the mass content of active carbon is 83.33% in the active carbon based composite catalyst.
The present invention uses heterogeneous cobaltosic oxide/graphite oxide/oxycellulose/active carbon/PMS catalyzing oxidizing degrading
System: using active carbon as carrier, supported cobaltosic oxide/graphite oxide/oxycellulose is catalyst, PMS is oxidant
System carries out catalyzing oxidizing degrading to methyl orange dye.
As the increase of PMS concentration can produce more SO4 -Come methyl orange dye waste water of degrading, therefore PMS concentration
Higher, methyl orange dye wastewater degradation is faster, but after PMS concentration increases to some amount, then increases PMS concentration, at increase
While managing cost, the degradation rate of methyl orange dye waste water is not obvious, and takes into account cost and treatment effeciency, most preferably
2m·mol/L。
As the increase of catalytic amount is so that having more catalytic active site catalysis PMS and then generating more in reaction system
SO4 -Come methyl orange dye waste water of degrading, therefore catalyst amounts are more, and the degradation rate of methyl orange dye waste water is got over
Fastly.But after catalyst charge increases to some amount, it is further added by the dosage of catalyst, the degradation speed of methyl orange dye waste water
Rate increase is not obvious, and takes into account cost and treatment effeciency, most preferably 1.2g/L.
Studies have shown that the high-level oxidation technology based on potentiometric titrations is the endothermic reaction, increasing temperature can significantly be mentioned
High reaction rate.However, increasing temperature will increase energy consumption, and then increase processing cost.Experiment shows degradation reaction in room
When carrying out under the conditions of temperature, degradation rate is just very high, therefore most preferably 25 DEG C.
For the present invention using PMS as oxidant, active carbon base complex is catalyst, degrades, is catalyzed to methyl orange
The absorption property and catalytic performance of agent are good, reusability is good and is easily recycled.
Compared with prior art, the beneficial effects of the present invention are:
Catalyst of the invention can be used at normal temperature, applied widely, this heterogeneous cobaltosic oxide/oxidation stone
Ink/oxycellulose/active carbon/PMS catalyzing oxidizing degrading system has high catalytic efficiency, and oxidability is strong, reusability
The advantages that good, particularly pertinent is that Catalyst Adsorption performance is good, and density is big, can be deposited to waste water bottom after the reaction was completed, be convenient for
Recycling.
Detailed description of the invention
Fig. 1 is oxidant dosages different in embodiment 2 to the data analysis chart of the wastewater degradation effect；
Fig. 2 is treatment of different temperature temperature in embodiment 3 to the data analysis chart of the wastewater degradation effect；
Fig. 3 is different catalysts dosage in embodiment 4 to the data analysis chart of the wastewater degradation effect；
Fig. 4 is that catalyst circulation uses the data analysis chart of six wastewater degradation effects in embodiment 5.
Specific embodiment
In order to make the present invention more obvious and understandable, hereby with preferred embodiment, and attached drawing is cooperated to be described in detail below.
Embodiment 1
Graphite oxide powder 200mg is added in n-hexyl alcohol (120mL), is formed it by ultrasonic 2h just evenly dispersed
Suspension, separately 1mmol cabaltous nitrate hexahydrate (is calculated by relative molecular mass 291.03 and is being dissolved in another just for 0.291g)
In hexanol (80mL), mixed after forming red solution with the suspension containing graphite oxide, and be stirred at room temperature
0.5h mixes two kinds of substances uniformly.Then mixture is heated at reflux 12h at 140 DEG C.After reaction by reactant
System is cooled to room temperature, centrifuge washing (centrifuge speed test is adjusted), and is washed repeatedly with ethyl alcohol to remove n-hexyl alcohol and wherein
Sundries, finally the product of acquisition is dried for standby in 60 DEG C of vacuum drying oven.
Sodium hydroxide, urea and deionized water are configured to 100g mixed solution according to 7: 12: 79 mass ratio, -10
Oxycellulose 2g is added at DEG C after sub-cooled 3h thereto, while quickly stirring 5min under 16,000rpm/min revolving speed
After be further continued for mixing slowly 2h, so that oxycellulose is sufficiently dissolved, obtain transparent oxycellulose solution later, continue
It stirs and is slowly warmed to room temperature and product is then centrifugated 10min by 8,000rpm, remove insoluble matter and bubble, obtain matter
Measure the oxycellulose solution that score is about 2%.Product (is lower than 10 DEG C) under cryogenic and saves backup.
The above-mentioned transparent Indium cellulose solution of 5g is slowly added to 6.25mL Co3O4/ GO (4mg/mL) suspension, stirring
Uniform and ultrasonic 10min is allowed to be sufficiently mixed, and mixed liquor is quickly stirred 30min under 16,000rpm/min revolving speed, continues slow
Speed stirring 8h obtains the uniform black slurries of color.It takes 10g black slurries to be added after 50g active carbon is stirred 3h and uses poly- four
Fluoride film filtering, with hydrochloric acid is adjusted to neutrality for PH before filtering, and dry 12h to get mass ratio is 1: 5 at 60 DEG C in air
Co3O4/ GO/ oxycellulose/active carbon composite catalyst.
Embodiment 2
The methyl orange solution of 100mL prepared 0.2mmol/L is added in five reactors, is separately added into
The PMS of 0.4mmol, 1mmol, 2mmol, 4mmol, 6mmol, 10mmol, then with 0.5mol/L's
NaHCO3Solution pH value is adjusted to 7 by buffer solution, and active carbon obtained in 0.12g embodiment 1 is added in each conical flask
Based composite catalyst, it is 25 DEG C that conical flask, which is put into thermostatic control oscillator vibration, and adjusts temperature, the constant temperature oscillation under given pace,
And start timing, the 5mL of interval sampling at regular intervals, and mixed with isometric quencher methanol solution, reaction is terminated, with
After filter.The corresponding absorbance of solution is finally measured at 486nm with UV-7504 type spectrophotometer.Every group of experiment repeats three
It is secondary to be averaged.Reaction result (C/C0Existing concentration is represented than upper initial concentration) as shown in Figure 1, showing that oxidant additional amount can
To largely effect on degradation effect, and the bigger degradation rate of additional amount is faster, finally takes into account cost and treatment effeciency, and selection is best
Oxidant additional amount is 2mmol.
Embodiment 3
The methyl orange solution of 100mL prepared 0.2mmol/L is added in four reactors, according to embodiment
2 as a result, the PMS of 2mmol is added in each conical flask, then use the NaHCO of 0.5mol/L3Buffer solution is by solution pH value
7 are adjusted to, active carbon based composite catalyst obtained in 0.12g embodiment 1 is added in each conical flask, respectively by conical flask
Being put into thermostatic control oscillator vibration and adjusting temperature is 15 DEG C, 25 DEG C, 40 DEG C, 60 DEG C, the constant temperature oscillation under given pace, and starting
Timing, the 5mL of interval sampling at regular intervals, and mixed with isometric quencher methanol solution, terminate reaction, subsequent mistake
Filter.The corresponding absorbance of solution is finally measured at 486nm with UV-7504 type spectrophotometer.Every group of experiment takes in triplicate
Average value.Reaction result (C/C0Existing concentration is represented than upper initial concentration) as shown in Fig. 2, showing that temperature can largely effect on drop
Effect is solved, and the higher degradation rate of temperature is faster, finally takes into account cost and treatment effeciency, selects optimum treatmenting temperature for 25
℃。
Embodiment 4
The methyl orange solution of 100mL prepared 0.2mmol/L is added in four reactors, according to embodiment
2 and example 3 as a result, the PMS of 2mmol is added in each conical flask, then use the NaHCO of 0.5mol/L3Buffer solution will be molten
Liquid pH value adjustment is 7, is added in the embodiment 1 of 0.08g, 0.1g, 0.12g, 0.14g, 0.16g and makes respectively in each conical flask
The active carbon based composite catalyst obtained, it is 25 DEG C that conical flask, which is put into thermostatic control oscillator vibration, and adjusts temperature, in given pace
Lower constant temperature oscillation, and start timing, the 5mL of interval sampling at regular intervals, and mixed with isometric quencher methanol solution,
Reaction is terminated, is then filtered.The corresponding absorbance of solution is finally measured at 486nm with UV-7504 type spectrophotometer.Every group
Experiment is averaged in triplicate.Reaction result (C/C0Existing concentration is represented than upper initial concentration) as shown in figure 3, showing to be catalyzed
Agent additional amount can largely effect on degradation effect, and the bigger degradation rate of additional amount is faster, finally take into account cost and processing effect
Rate selects optimum catalyst additional amount for 1.2g/L.
Embodiment 5
The methyl orange solution of 100mL prepared 0.2mmol/L is added in six reactors, according to embodiment
2 and example 3 as a result, the PMS of 2mmol is added in each conical flask, then use the NaHCO of 0.5mol/L3Buffer solution will be molten
Liquid pH value adjustment is 7, and active carbon based composite catalyst obtained in the embodiment 1 of 0.12g is added in each conical flask respectively,
It is 25 DEG C that conical flask, which is put into thermostatic control oscillator vibration, and adjusts temperature, the constant temperature oscillation under given pace, and starts timing, often
5mL is sampled from a wherein constant conical flask every certain time interval, and is mixed with isometric quencher methanol solution,
Reaction is terminated, is then filtered.The corresponding absorbance of solution is finally measured at 486nm with UV-7504 type spectrophotometer.Reaction
After by the catalyst collection of each parallel reaction, then washed with centrifugation, ethyl alcohol, vacuum drying etc. obtains drying pure catalysis
Agent, then respectively weigh again 0.12g amount be added five conical flasks in, carry out subsequent circular response, so circulation 5 times.Finally
It once weighs 0.12g catalyst to be only added in a conical flask, other steps are same as above.Reaction result (C/C0Represent existing concentration
Than upper initial concentration) as shown in figure 4, Acid Orange II remains to reach 100% degradation effect in a short time after 5 circulations
Fruit shows that rear catalyst, which is used for multiple times, still maintains higher catalytic activity, degradable still to complete in 14min.
Claims (10)
1. a kind of preparation method for the active carbon based composite catalyst for being catalyzed persulfate degradation of dye methyl orange, feature exist
In first cobaltosic oxide being loaded on graphite oxide, then the graphite oxide of supported cobaltosic oxide is answered with oxycellulose
Close, then by compound with active carbon is compound prepares active carbon based composite catalyst, be finally added into the water containing methyl orange
Potassium Monopersulfate adjusts pH value, and active carbon based composite catalyst is added and is degraded.
2. the preparation side of the active carbon based composite catalyst of catalysis persulfate degradation of dye methyl orange as described in claim 1
Method, which is characterized in that the active carbon based composite catalyst the preparation method comprises the following steps:
Step 1: graphite oxide powder is added in n-hexyl alcohol, evenly dispersed suspension is formed it by ultrasound, separately will
Cabaltous nitrate hexahydrate is dissolved in another n-hexyl alcohol, is mixed after forming red solution with the suspension containing graphite oxide
It closes, and being stirred at room temperature mixes two kinds of substances uniformly, mixture is then heated at reflux 12h, reaction knot at 140 DEG C
Reaction system is cooled to room temperature, centrifuge washing after beam, and is washed repeatedly to remove n-hexyl alcohol and sundries therein, most with ethyl alcohol
The product of acquisition is dried for standby in 60 DEG C of vacuum drying oven afterwards；
Step 2: high-speed stirred dissolves oxycellulose to sodium hydroxide/thiocarbamide/urea liquid at low temperature, transparent oxygen is obtained
Product is then removed insoluble matter and bubble by high speed centrifugation by cellulose solution, and cobaltosic oxide/graphite oxide is compound
Object powder ultrasonic disperses 1h, is uniformly mixed with cellulose solution, mixed liquor is mixed with active carbon again, finally uniformly mixed slurry
Liquid is filtered using polytetrafluoroethylene film, with hydrochloric acid pH is adjusted to neutrality before filtering, in air at 60 DEG C dry 12h to get work
Property charcoal based composite catalyst.
3. the preparation side of the active carbon based composite catalyst of catalysis persulfate degradation of dye methyl orange as described in claim 1
Method, which is characterized in that the additional amount of the Potassium Monopersulfate is 0.4-10mmol/L.
4. the preparation side of the active carbon based composite catalyst of catalysis persulfate degradation of dye methyl orange as described in claim 1
Method, which is characterized in that the additional amount of the active carbon based composite catalyst is 0.8-1.6g/L.
5. the preparation side of the active carbon based composite catalyst of catalysis persulfate degradation of dye methyl orange as described in claim 1
Method, which is characterized in that the pH value is 4-10.
6. the preparation side of the active carbon based composite catalyst of catalysis persulfate degradation of dye methyl orange as described in claim 1
Method, which is characterized in that the temperature of the degradation is 15-60 DEG C；Degradation time is 2-14min.
7. the preparation side of the active carbon based composite catalyst of catalysis persulfate degradation of dye methyl orange as described in claim 1
Method, which is characterized in that the initial concentration of the methyl orange is 0.1-1mmol/L.
8. the preparation side of the active carbon based composite catalyst of catalysis persulfate degradation of dye methyl orange as described in claim 1
Method, which is characterized in that the additional amount of the Potassium Monopersulfate is 2mmol/L；The additional amount of active carbon based composite catalyst is
1.2g/L；PH value is 7；Degradation temperature is 25 DEG C, degradation time 8min；The initial concentration of methyl orange is 0.2mmol/L in water.
9. a kind of multiple using the active carbon base for being catalyzed persulfate degradation of dye methyl orange described in claim 1-8 any one
Close the active carbon based composite catalyst of the catalysis persulfate degradation of dye methyl orange of the preparation method preparation of catalyst.
10. the active carbon based composite catalyst of catalysis persulfate degradation of dye methyl orange as claimed in claim 9, feature
It is, the mass content of active carbon is 83.33% in the active carbon based composite catalyst.
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| CN108298668A (en) * | 2018-03-31 | 2018-07-20 | 苏州科技大学 | A kind of method of azo dyes gold orange-G in degrading waste water |
| CN112892553B (en) * | 2021-02-04 | 2022-02-11 | 中南大学 | Oxygen-enriched vacancy cobaltosic oxide/manganese slag composite ternary metal magnetic catalyst and preparation method and application thereof |
| CN115259499A (en) * | 2022-08-17 | 2022-11-01 | 生态环境部南京环境科学研究所 | By using Co 2+ Method for degrading methyl orange by catalyzing potassium peroxymonosulfate |
| CN117019118B (en) * | 2023-10-08 | 2024-01-05 | 西安金沃泰环保科技有限公司 | Filtering material for benzene series waste gas and preparation method thereof |
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