CN110369708A - A kind of method that aging is modified the preparation method of Zero-valent Iron and is modified Zero-valent Iron degradating chloro organic pollutant using aging - Google Patents
A kind of method that aging is modified the preparation method of Zero-valent Iron and is modified Zero-valent Iron degradating chloro organic pollutant using aging Download PDFInfo
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- CN110369708A CN110369708A CN201910680040.8A CN201910680040A CN110369708A CN 110369708 A CN110369708 A CN 110369708A CN 201910680040 A CN201910680040 A CN 201910680040A CN 110369708 A CN110369708 A CN 110369708A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/46—Removing components of defined structure
- B01D53/68—Halogens or halogen compounds
- B01D53/70—Organic halogen compounds
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/14—Treatment of metallic powder
- B22F1/145—Chemical treatment, e.g. passivation or decarburisation
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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
- C02F1/58—Treatment of water, waste water, or sewage by removing specified dissolved compounds
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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
- C02F2101/36—Organic compounds containing halogen
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Abstract
The invention belongs to chemical fields, relate to the use of the method for modified Zero-valent Iron degradable organic pollutant.A kind of preparation method of the modified Zero-valent Iron of aging, the following steps are included: (1) room temperature is 18 DEG C, 250ml NaAc_HAc buffer solution is added into 250ml reaction flask, controls its pH between 5.5-6.5, logical nitrogen makes dissolved oxygen be reduced to 0,1g zeroth order iron powder is added, the sodium sulfide solution of 0.5ml1M is then added in ultrasound 5 minutes, is placed in shaking table 200rpm and shakes 5-30 minutes, it is shaken up after taking-up, filter and is freeze-dried 1 hour up to modified Zero-valent Iron product；(2) modified Zero-valent Iron product is placed in 15-25 DEG C of nitrogen atmosphere, is placed for 24 hours；Natural aging 3-10 days in air are then taken out, the modified Zero-valent Iron of aging is made.The present invention has broken the understanding prejudice that Zero-valent Iron aging inactivates in traditional technology using the method for the modified Zero-valent Iron degradating chloro organic pollutant of aging, provides one kind by aging process and improves Zero-valent Iron reactivity, reduces the new approaches of storage cost.
Description
Technical field
The invention belongs to chemical fields, relate to the use of the method for modified Zero-valent Iron degradable organic pollutant.
Background technique
Chlorinatedorganic object is that the hydrogen atom in a type organic is substituted by a chlorine atom both, and is using carbon or hydrocarbon as skeleton and chlorine phase
In conjunction with series of elements organic compound general name.Its is fat-soluble good, and chlorine atom, which increases the flammable of its compound, to be reduced.With
Different gas, liquid, solid states exists.It is widely used in the intermediate, solvent and pesticide etc. of synthetic.Solvent emanation and its system
Product waste often enters atmosphere and ocean, causes environmental pollution.Vinyl chloride monomer carbon tetrachloride, chloroform etc. have liver very strong
Toxicity, some have carcinogenicity.Some organochlorine compounds are highly stable in the environment, such as Polychlorinated biphenyls (PCD), DDT and six or six
Six etc., self-stopping technology produces so far, still can detect that higher residue in water body, bed mud and organism.It is fat-soluble due to having,
Metabolism slowly, by food chain concentration, accumulation, mainly causes long-term chronic poisonous effect in vivo.In homologue
With increasing for chlorine atom, toxicity enhances, and related in its chemical structure.Aliphatic chloride easily causes in terms of damage to liver
Fatty liver, aromatic chlorinated object easily lead to the lesion characterized by yellow atrophy.Most chlorohydrocarbons are non-ignitable, but in flame or add
It can be decomposed when hot, the phosgene for releasing hydrochloric acid and severe toxicity enters atmosphere.
Zero-valent Iron is because of the features such as environmental-friendly, nontoxic, rich content, the strong reproducibility and extensive pass by researcher
Note, is increasingly taken seriously in water treatment field.Although zero-valent iron technology has been obtained comparing and has been widely applied, there is also prominent
Out the shortcomings that.For example Zero-valent Iron, due to air oxidation surface passivation, will form the oxidation of uneven thickness during preparation
Film.The Zero-valent Iron prepared also can lose reactivity with the aging of time in air and water environment.Existing research person is equal
It confirms over time, Zero-valent Iron aging in air or water can reduce the reactivity of Zero-valent Iron or even lose Zero-valent Iron
It is living.Cause the zeroth order iron material shelf-life short due to inactivation aging inactivation, affects the application and flexibility of its industry.
Quickening reaction rate is generallyd use in the prior art, shortens the means such as reaction process to make Zero-valent Iron as far as possible in short-term
Between exposure in the environment, avoid the formation of oxidation film, keep its activity.There has been no zeroth order iron material is modified to keep
Or improve the report of its reactivity.
Summary of the invention
The object of the present invention is to provide the methods that a kind of pair of aging zeroth order iron material is modified, and provide to use simultaneously and change
The method of aging Zero-valent Iron material degradation solution organo-chlorine pollutant after property.
To achieve the goals above, the technical solution adopted by the present invention is that: a kind of preparation method of the modified Zero-valent Iron of aging,
The following steps are included:
(1) room temperature is 18 DEG C, and 250ml NaAc_HAc buffer solution is added into 250ml reaction flask, controls its pH in 5.5-
Between 6.5, logical nitrogen makes dissolved oxygen be reduced to 0, and 1g zeroth order iron powder is added, and the vulcanized sodium of 0.5ml1M is then added in ultrasound 5 minutes
Solution is placed in shaking table 200rpm and shakes 5-30 minutes, shakes up after taking-up, filters and is freeze-dried 1 hour up to modified zeroth order
Iron product；
(2) modified Zero-valent Iron product is placed in 15-25 DEG C of nitrogen atmosphere, is placed for 24 hours；Then take out natural aging in air
3-10 days, the modified Zero-valent Iron of aging is made.
As a further improvement of the present invention, the Zero-valent Iron that the zeroth order iron powder is partial size 70-80 microns.
As a further improvement of the present invention, the concentration of nitrogen is 55%-95% in the nitrogen atmosphere.
As a further improvement of the present invention, the humidity of nitrogen is 30%-70% in the nitrogen atmosphere.
As a further improvement of the present invention, in air natural aging when air humid control in 30%-60%.
As a further improvement of the present invention, in air natural aging when air temperature control at 15-25 DEG C.
Second object of the present invention is achieved through the following technical solutions: a kind of to utilize the modified Zero-valent Iron degradating chloro of aging
The method of organic pollutant, comprising the following steps:
At room temperature, 500 mL deionized waters, mechanical agitator stirring are added into 500 mL reaction vessels, control revolving speed is 100-
400 r/min, it is 25 ± 2 DEG C that thermostat water bath, which keeps whole reaction temperature, and the modified Zero-valent Iron of 0.4g/L aging is then added
Grain；Organo-chlorine pollutant chloromycetin wastewater is added, adjusts initial pH=3-7, reaction can remove the organic dirt of chloro in 2-5 hours
Contaminate object.
As a further improvement of the present invention, chlorinatedorganic concentration is 25mg/L in reaction system.
As a further improvement of the present invention, initial p H=3-7 is adjusted using sulfuric acid or citric acid solution.
As further improvement of the invention, initial pH=3 are adjusted using citric acid solution.
Aging of the invention is modified the method for Zero-valent Iron and utilizes the modified Zero-valent Iron degradating chloro organic pollutant of aging
Then modified Zero-valent Iron is carried out aging process, the modification Zero-valent Iron after aging again by being first modified to zeroth order iron material by method
The reactivity of material enhances, and the ability of degradating chloro organic pollutant improves.The present invention has broken Zero-valent Iron in traditional technology
The understanding prejudice of aging inactivation provides one kind by aging process and improves Zero-valent Iron reactivity, when extending the storage of material
Between and reduce storage cost new approaches.
Detailed description of the invention
Fig. 1 is the modification zeroth order iron material of different days of ageing, is compared the removal rate of chloramphenicol, ordinate is chloramphenicol
Degradation rate, abscissa are the reaction time；
Fig. 2 is that the modified Zero-valent Iron of aging compares the removal rate of chloramphenicol in different acid for adjusting pH, SZVI-US-CA(3) it is lemon
Lemon acid for adjusting pH, SZVI-US-SA(3) it is sulphur acid for adjusting pH；
Fig. 3 is that the modified Zero-valent Iron of aging compares the removal rate of chloramphenicol in the different initial pH of same acid adjusting, SZVI-
US-SA(3), it is 3,5,7 that (5), (7), which respectively indicate pH,；
Fig. 4 is that the modification zeroth order iron material of aging and not aged modified zeroth order iron material compare the removal rate of chloramphenicol:
SZVI-CA be aging modification+citric acid, ZVI-CA is unaged modification+citric acid, SZVI-SA be aging modification+sulfuric acid,
ZVI-SA is unaged modification+sulfuric acid；
The XPS image of the Fe2p for the modification Zero-valent Iron that Fig. 5 is aging 7 days.
Specific embodiment
The method of Zero-valent Iron is modified to aging of the invention with reference to the accompanying drawings and examples and utilizes the modified zeroth order of aging
The method of iron degradating chloro organic pollutant is described in detail and illustrates, so that those skilled in the art can preferably manage
Solve technical solution of the present invention and technical effect.
Embodiment 1: the present embodiment provides a kind of by the modified zeroth order iron material of aging, improves material activity, utilizes simultaneously
The modified Zero-valent Iron of the aging is degraded the method containing chloromycetin wastewater under aerobic conditions.
Room temperature is 18 DEG C, and 250ml NaAc_HAc buffer solution is added into 250ml reaction flask, controls its pH in 5.5-
Between 6.5, logical nitrogen makes dissolved oxygen be reduced to 0, and 70-80 microns of 1g partial size of zeroth order iron powder, ultrasound 5 minutes, superonic spectrum is added
For 40kHz.
The sodium sulfide solution of 0.5ml1M is then added, is placed in shaking table 200rpm and shakes 5-30 minutes, shaken up after taking-up, taken out
Filter is simultaneously modified Zero-valent Iron product in freeze-drying 1 hour for -40 DEG C to obtain the final product.
Above-mentioned material is placed in 25 DEG C of nitrogen atmospheres, control humidity is 35%, is placed for 24 hours.It then takes out in air,
Keeping air themperature is 20 DEG C, air humidity 35%, and aging 0,1,3,5,7,9 day respectively, the modified Zero-valent Iron of aging is made.
At room temperature, 500 mL deionized waters, mechanical agitator stirring, control are separately added into 6 500 mL reaction vessels
Revolving speed processed is 100 r/min, and it is 25 ± 2 DEG C that thermostat water bath, which keeps whole reaction temperature, then respectively into 6 reaction vessels
The modification zero-valent iron particle that 0.4g/L days of ageing is 0,1,3,5,7,9 day, modification Zero-valent Iron (the i.e. aging without aging is added
Number of days is 0) as control；Chloromycetin wastewater is added, the concentration for controlling chloramphenicol in reaction vessel is 25 mg/L, and sulfuric acid is added dropwise
Initial p H=3 are adjusted, the degradation situation of 3 hours observation chloramphenicol is reacted.
As a result as shown in Figure 1, the modification zeroth order iron material of aging 0,1,3,5,7,9 day, reacting 150 minutes can different journey
Degree removes most of chloramphenicol.But ageing time is less than 3 days modification zeroth order iron materials, remove the effect of chloramphenicol with without
The modification Zero-valent Iron differences in materials of aging is little.Aging 3 days or more modification zeroth order iron materials, the effect for removing chloramphenicol are equal
Better than the modification zeroth order iron material without aging, wherein the 7th day modification Zero-valent Iron of ageing time can be gone in 150 min
Except 80.7 % or more of chloramphenicol, removal effect is apparently higher than other days of ageing.Also, the present embodiment also found, ageing time
More than 10 days modification zeroth order iron material removal chloramphenicol effect substantially with the modification zeroth order iron material without aging maintain an equal level or
It is worse.Therefore, the too short or too long modification zeroth order iron material of ageing time, the effect for removing chloramphenicol are undesirable.
The XPS image of the Fe2p of aging 7 days modification Zero-valent Irons is as shown in figure 5, the peak within the scope of 712-713 is Fe3O4
Peak, Fe3O4The conduction of electronics can be enhanced by being a kind of strong electronic conductor as a kind of conductive oxide, can speed up iron core to table
The electron transmission in face；It is possible to promote absorption simultaneously, increases the adsorption site of pollutant, so that contaminant degradation efficiency is improved,
This may be material in aging the 7th day foundation with higher removal organo-chlorine pollutant performance.
Embodiment 2: room temperature is 18 DEG C, and 250ml NaAc_HAc buffer solution, control are added into 250ml reaction flask
For its pH between 5.5-6.5, logical nitrogen makes dissolved oxygen be reduced to 0, and 70-80 microns of 1g partial size of zeroth order iron powder, 5 points of ultrasound is added
The sodium sulfide solution of 0.5ml1M is then added in clock, is placed in shaking table 200rpm and shakes 5-30 minutes, shake up after taking-up, filters and cold
Dry 1 hour is lyophilized up to modified Zero-valent Iron product.
Modified Zero-valent Iron is placed in 15-25 DEG C of nitrogen atmosphere, control humidity is 60%, is placed for 24 hours.Then take out in sky
In gas, keeping air themperature is 20 DEG C, air humidity 35%, and aging 7 days, the modified Zero-valent Iron of aging is made.
At room temperature, 500 mL deionized waters, mechanical agitator stirring, control are separately added into two 500 mL reaction vessels
Revolving speed processed is 100 r/min, and it is 25 ± 2 DEG C that thermostat water bath, which keeps whole reaction temperature, is then added 0.4g/L aging 7 days
Modified Micron zero-valent iron particle；Chloromycetin wastewater is added, the concentration for controlling chloramphenicol in reaction vessel is 25 mg/L；Two anti-
It answers and sulfuric acid and initial pH=3 of citric acid adjusting is added dropwise in container respectively, react the degradation situation of observation in 3 hours.Lemon acid for adjusting pH
The modified Zero-valent Iron of aging can remove 99.7 % or more of chloramphenicol in 60 min, and removal effect is higher than sulphur acid for adjusting pH, as a result
As shown in Figure 2.
Embodiment 3: room temperature is 18 DEG C, and 250ml NaAc_HAc buffer solution, control are added into 250ml reaction flask
For its pH between 5.5-6.5, logical nitrogen makes dissolved oxygen be reduced to 0, and 70-80 microns of 1g partial size of zeroth order iron powder, 5 points of ultrasound is added
The sodium sulfide solution of 0.5ml1M is then added in clock, is placed in shaking table 200rpm and shakes 5-30 minutes, shake up after taking-up, filters and cold
Dry 1 hour is lyophilized up to modified Zero-valent Iron product.
Modified Zero-valent Iron is placed in 25 DEG C of nitrogen atmospheres, control humidity is 80%, is placed for 24 hours.Then take out in air
In, keeping air themperature is 20 DEG C, air humidity 35%, and aging 7 days, the modified Zero-valent Iron of aging is made.
At room temperature, 500 mL deionized waters, mechanical agitator stirring, control are separately added into 3 500 mL reaction vessels
Revolving speed processed is 100 r/min, and it is 25 ± 2 DEG C that thermostat water bath, which keeps whole reaction temperature, is then added 0.4g/L aging 7 days
Modified zero-valent iron particle；Chloromycetin wastewater is added, the concentration for controlling chloramphenicol in reaction vessel is 25 mg/L, 3 reaction vessels
Sulfuric acid is inside added dropwise respectively and adjusts initial pH=3, pH=5, pH=7, reacts the degradation situation of observation in 3 hours.The aging of sulphur acid for adjusting pH=3
Zero-valent Iron can remove 99.7 % or more of chloramphenicol in 60 min, and removal effect is higher than under other pH value conditions, as a result such as Fig. 3
It is shown.
Embodiment 4: room temperature is 18 DEG C, and 250ml NaAc_HAc buffer solution is added into 250ml reaction flask, controls it
For pH between 5.5-6.5, logical nitrogen makes dissolved oxygen be reduced to 0, and 1g zeroth order iron powder is added, and 0.5ml1M is then added in ultrasound 5 minutes
Sodium sulfide solution, be placed in shaking table 200rpm and shake 5-30 minutes, shaken up after taking-up, filter and be freeze-dried 1 hour and change to obtain the final product
Property Zero-valent Iron product.
Above-mentioned material is placed in 20 DEG C of nitrogen atmospheres, control humidity is 55%, is placed for 24 hours.It then takes out in air,
Keeping air themperature is 25 DEG C, air humidity 35%, and aging 7 days, the modified Zero-valent Iron of aging is made.
At room temperature, 500 mL deionized waters, mechanical agitator stirring, control are separately added into 4 500 mL reaction vessels
Revolving speed processed is 100 r/min, and it is 25 ± 2 DEG C that thermostat water bath, which keeps whole reaction temperature, then respectively into 2 reaction vessels
The modification zero-valent iron particle of aging is added, the modification zero-valent iron particle without aging is in addition added in 2 reaction vessels；4 anti-
It answers and chloromycetin wastewater is added in container, the concentration for controlling chloramphenicol in reaction vessel is 25 mg/L, to the modification of 2 agings
Citric acid is added dropwise in Zero-valent Iron reaction system respectively and sulfuric acid adjusts initial pH=3,2 not aged Zero-valent Iron reaction systems
Citric acid is added dropwise respectively and sulfuric acid adjusts initial pH=3, reacts the degradation situation of observation in 3 hours.As seen from Figure 4, to chloramphenicol
Degradation rate are as follows: aging modification+citric acid > unaged modification+citric acid > aging modification+sulfuric acid > unaged modification+sulfuric acid.Always
Change the time the 7th day modification Zero-valent Iron citric acid control pH under the conditions of can be removed in 60 min 99.3 % of chloramphenicol with
On, removal effect is substantially better than the modified zeroth order iron material of aging of sulfuric acid control pH and the zeroth order iron material of unaged modification,
The modification Zero-valent Iron and citric acid for illustrating aging have synergistic effect in removal organo-chlorine pollutant.
Claims (10)
1. a kind of preparation method of the modified Zero-valent Iron of aging, which comprises the following steps: (1) room temperature be 18 DEG C, to
250ml NaAc_HAc buffer solution is added in 250ml reaction flask, controls its pH between 5.5-6.5, logical nitrogen makes to dissolve
Oxygen is reduced to 0, and 1g zeroth order iron powder is added, and the sodium sulfide solution of 0.5ml1M is then added in ultrasound 5 minutes, is placed in shaking table 200rpm shake
It swings 5-30 minutes, is shaken up after taking-up, filtered and be freeze-dried 1 hour up to modified Zero-valent Iron product；
(2) modified Zero-valent Iron product is placed in 15-25 DEG C of nitrogen atmosphere, is placed for 24 hours；Then take out natural aging in air
3-10 days, the modified Zero-valent Iron of aging is made.
2. the preparation method of the modified Zero-valent Iron of aging according to claim 1, which is characterized in that nitrogen in the step (2)
The concentration of gas is 55%-95%.
3. the preparation method of the modified Zero-valent Iron of aging according to claim 1, which is characterized in that nitrogen in the step (2)
The humidity of gas is 30%-70%.
4. the preparation method of the modified Zero-valent Iron of aging according to claim 1, which is characterized in that the step (2) is hollow
The humid control of gas is in 30%-60%.
5. the preparation method of the modified Zero-valent Iron of aging according to claim 1, which is characterized in that the step (2) is hollow
The temperature of gas is controlled at 15-25 DEG C.
6. the preparation method of the modified Zero-valent Iron of aging according to claim 1-5, which is characterized in that described zero
The Zero-valent Iron that valence iron powder is partial size 70-80 microns.
7. a method of utilize the modified Zero-valent Iron degradating chloro organic pollutant of aging, which comprises the following steps:
At room temperature, 500 mL deionized waters, mechanical agitator stirring are added into 500 mL reaction vessels, control revolving speed is 100-
400 r/min, it is 25 ± 2 DEG C that thermostat water bath, which keeps whole reaction temperature, and the modified Zero-valent Iron of 0.4g/L aging is then added；Add
Enter chlorinatedorganic pollutant effluents, adjust initial pH=3-7,2-5 hour of reaction can remove organo-chlorine pollutant.
8. the method according to claim 7 using the modified Zero-valent Iron degradating chloro organic pollutant of aging, feature exist
In: chlorinatedorganic concentration is 25 mg/L in reaction system.
9. the method according to claim 7 using the modified Zero-valent Iron degradating chloro organic pollutant of aging, feature exist
In: initial pH=3-7 is adjusted using sulfuric acid or citric acid solution.
10. the method according to claim 9 using the modified Zero-valent Iron degradating chloro organic pollutant of aging, feature exist
In: initial pH=3 are adjusted using citric acid.
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