CN108911101A - A method of based on the efficient heavy-metal ion removal of ball milling oxalic acid Zero-valent Iron - Google Patents
A method of based on the efficient heavy-metal ion removal of ball milling oxalic acid Zero-valent Iron Download PDFInfo
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- CN108911101A CN108911101A CN201810662373.3A CN201810662373A CN108911101A CN 108911101 A CN108911101 A CN 108911101A CN 201810662373 A CN201810662373 A CN 201810662373A CN 108911101 A CN108911101 A CN 108911101A
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- zero
- valent iron
- oxalic acid
- ball milling
- metal ion
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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
- C02F1/70—Treatment of water, waste water, or sewage by reduction
- C02F1/705—Reduction by metals
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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
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
Abstract
The present invention relates to a kind of methods based on the efficient heavy-metal ion removal of ball milling oxalic acid Zero-valent Iron.This method is：Ball milling oxalic acid Zero-valent Iron is added in the aqueous solution containing heavy metal ion, the removal of heavy metal ion is carried out.The method of the ball milling oxalic acid Zero-valent Iron is that oxalic acid and Zero-valent Iron are prepared by solid-phase ball milling method, and the ability of heavy-metal ion removal significantly increases, and solves the problems, such as that Zero-valent Iron heavy-metal ion removal activity is low.The improvement that is simple, at low cost, environmental-friendly, can be widely used for various heavy polluted underground water of the preparation method of oxalic acid Zero-valent Iron provided by the invention.
Description
Technical field
The invention belongs to Environmental Chemistry fields, and in particular to be based on the efficient heavy-metal ion removal of ball milling oxalic acid Zero-valent Iron
Method, be applicable to the processing of the fields such as printing and dyeing, industry waste water.
Background technique
Dosage is continuous in industrial or agricultural, science and technology, daily life for heavy metal (chromium, arsenic, lead, cadmium, copper, nickel, zinc, tin, mercury etc.)
Increase, and can be discharged into environment with various channels, Heavy Metals In Environment total amount is caused to continue to increase.Heavy metal pollution is easily long-pending
Tired, irreversible, toxicity is big, metabolism slowly and easily enrichment the features such as, seriously endanger human health.Therefore, develop green high-efficient
Heavy metal pollution control technology is extremely urgent.
Relative to other heavy metal pollution recovery techniques, zero-valent iron technology has environmental-friendly, removal various heavy etc.
Feature is widely used in the improvement of waste water and polluted underground water over 20 years.But zeroth order iron surface is easy to by water and oxygen institute
Oxidation, one layer of ferriferous oxide of Surface Creation form unique core shell architecture.And the official of the thickness of ferriferous oxide shell and its surface
The absorption and reduction for all affecting heavy metal can be rolled into a ball, the thickness effect electron transfer rate of oxide layer aoxidizes the function of layer surface
Group influences the absorption of heavy metal, to decide that electronics that Zero-valent Iron is transmitted out is used for the ratio of reducing heavy metal, i.e. electronics
Selectivity.Researcher has developed a variety of methods to eliminate the negative effect of shell, for example, using pickling, reducing agent reduction and
The modes (part) such as ultrasound removing remove Zero-valent Iron surface crust, or apply the corrosion rate etc. that low-intensity magnetic field accelerates Zero-valent Iron.This
A little methods reduce the thickness of oxide layer simply by pretreatment, but oxide layer generates again during removing removing heavy metals,
So being also difficult to solve the problems, such as that Zero-valent Iron removal heavy metal activity is not high by the removal of oxide layer.
Summary of the invention
The technical problem to be solved by the present invention is to provide a kind of based on ball milling oxalic acid in view of the deficiencies of the prior art
The method of the efficient heavy-metal ion removal of Zero-valent Iron.
The present invention be solve the problems, such as it is set forth above used by technical solution be：
A method of based on the efficient heavy-metal ion removal of ball milling oxalic acid Zero-valent Iron, ball milling oxalic acid Zero-valent Iron is added
Enter in the aqueous solution containing heavy metal ion, carries out the removal of heavy metal ion, the ball milling oxalic acid Zero-valent Iron is by oxalic acid
It is prepared with Zero-valent Iron by solid-phase ball milling method.
According to the above scheme, it is washed after the oxalic acid and Zero-valent Iron ball milling, vacuum drying obtains oxalic acid Zero-valent Iron.It is described
Washing be washing after alcohol wash.
According to the above scheme, the oxalic acid accounts for the molar percentage of Zero-valent Iron and is：0.2-2.0%.
According to the above scheme, the Ball-milling Time：0.5-5h, rotational speed of ball-mill 300-800r/min.
According to the above scheme, the partial size, pattern of the Zero-valent Iron, purity and resting period no requirement (NR).Zero-valent Iron can be micron
Grade, can also be nanoscale.
According to the above scheme, the oxalic acid purity is technical grade or more.
According to the above scheme, the dosage of the ball milling oxalic acid Zero-valent Iron is 1-5g/L.
According to the above scheme, the concentration of heavy metal ion is 2-50ppm, and reaction temperature is 10-30 DEG C, and reaction pH is 4-
8。
According to the above scheme, it is shaken in removal process with shaking table, comes into full contact with heavy metal ion and Zero-valent Iron.Using shaking table
Shaking purpose is to come into full contact with heavy metal ion and Zero-valent Iron.If preferable effect can also be obtained without concussion.
According to the above scheme, the heavy metal includes but is not limited to chromium, mercury, silver, lead, nickel.
Technical principle of the invention (see Fig. 1)：
Zeroth order iron surface covers one layer of hydroxyl, and poor to the adsorption capacity of heavy metal ion, more Zero-valent Irons are by water and oxygen
Gas is aoxidized, so Zero-valent Iron surface hydroxyl is unfavorable for the absorption to heavy metal ion.After oxalic acid and Zero-valent Iron ball-milling treatment,
Oxalate replaces surface hydroxyl and with chemical bonds to zeroth order iron surface, and this in-situ modification is in the ironing surface oxalate of zeroth order
Zeroth order iron surface can be stable in the presence of.Zeroth order iron surface oxalic acidization can promote the adsorption capacity to heavy metal ion, to mention
The electronics of high Zero-valent Iron is used for the ratio of reducing heavy metal ion, and the electronics for reducing Zero-valent Iron reacts consumption with water or oxygen
Amount, is achieved in the efficient removal of heavy metal ion.Experiments verify that being used to remove different heavy metal ion all has high work
Property.
The advantage of the invention is that：
1, the present invention is based on the efficient heavy-metal ion removal of ball milling oxalic acid Zero-valent Iron, method is simple, easy to operate, can be obvious
Promote the removal of heavy metal ion.
2, Zero-valent Iron is cheap, environmental-friendly, can be widely used in practical Heavy Metal Pollution Control.
3, method of the invention has universal removal ability to different heavy metal ion.
Detailed description of the invention
The preparation principle figure of Fig. 1 ball milling oxalic acid Zero-valent Iron；
1 ball milling of Fig. 2 embodiment prepares oxalic acid Zero-valent Iron and Zero-valent Iron except directly addition oxalic acid activity comparison during chromium
Figure；
Cr VI effect picture in 2 ball milling oxalic acid Zero-valent Iron pollution administration water body of Fig. 3 embodiment；
Mercury effect picture in 3 ball milling oxalic acid Zero-valent Iron polluted-water of Fig. 4 embodiment；
Silver-colored effect picture in 4 ball milling oxalic acid Zero-valent Iron pollution administration water body of Fig. 5 embodiment；
Lead effect picture in 5 ball milling oxalic acid Zero-valent Iron pollution administration water body of Fig. 6 embodiment；
Nickel effect picture in 6 ball milling oxalic acid Zero-valent Iron pollution administration water body of Fig. 7 embodiment；
Specific embodiment
Carry out the summary of the invention that the present invention will be described in detail below by specific implementation case, described specific embodiment is only used
To explain the present invention, it is not intended to limit the present invention.
1 ball milling of embodiment prepares oxalic acid Zero-valent Iron and Zero-valent Iron except addition oxalic acid effect contrast figure direct during chromium
5.6g Zero-valent Iron (partial size is up to 80 μm) and 0.126g oxalic acid (containing two water) are put into ball grinder, revolving speed is
550r/min, Ball-milling Time 2h, the alcohol of sample washing later wash vacuum drying and obtain oxalic acid Zero-valent Iron Fe/Ox (n=
1.0%).Chromate waste water, pH value of solution 6.5 are simulated with the potassium bichromate solution 30mL that hexavalent chromium concentration is 20mg/L, temperature is
25 DEG C, Fe/Ox sample 0.1g is added, is put into the shaking table that revolving speed is 150r/min, periodically samples, spectrophotometry surveys solution sexavalence
Chromium concn.As control experiment, by the 0.097g Fe contained in theoretical amount in 0.1g Fe/Ox (n=1.0%) sample and
0.003g oxalic acid (concentration of oxalic acid 0.79mmol/L) is added in chrome liquor, and adjusting pH value of solution is 6.5.As further check experiment,
Different oxalic acid amount (system medium-height grass acid concentration is respectively 0.01,0.1mol/L) conducts are added again while 0.1g Zero-valent Iron is added
Control experiment, adjusting pH value of solution is 6.5, and other conditions are constant, as a result see Fig. 2.Oxalic acid Zero-valent Iron 120min of the invention is almost
Completely remove chromium；And directly 0.003g oxalic acid is added except in chromium system, reaction 120min only eliminates about 10%；With oxalic acid
Amount is sequentially increased, except chromium activity is enhanced, but still substantially less than oxalic acid Zero-valent Iron.
The above-mentioned oxalic acid Zero-valent Iron for absolutely proving the present invention and preparing by using oxalic acid and Zero-valent Iron solid-phase ball milling method, can
Realize the efficient removal of chromium.
Cr VI effect picture in 2 ball milling oxalic acid Zero-valent Iron pollution administration water body of embodiment
By 5.6g Zero-valent Iron (partial size is up to 160 μm) and different oxalic acid amounts, (molar ratio of oxalic acid and Zero-valent Iron is followed successively by：
0%, 0.2%, 0.5%, 1.0%, 2.0%) it is put into ball grinder, revolving speed 550r/min, Ball-milling Time 2h, sample washing
Alcohol washes vacuum drying and obtains oxalic acid Zero-valent Iron, i.e. Fe/Ox (n=0.0%, 0.2%, 0.5%, 1.0%, 2.0%).Use sexavalence
The potassium bichromate solution 30mL that chromium concn is 20mg/L simulates chromate waste water, and pH value of solution 5.2, temperature is 30 DEG C, and Fe/Ox is added
Sample 0.1g is put into the shaking table that revolving speed is 150r/min, periodically samples, and spectrophotometry surveys solution hexavalent chromium concentration, as a result sees
Fig. 3.Non- oxalic acid Zero-valent Iron only eliminates 10% in 120min, and oxalic acid Zero-valent Iron is greatly improved except chromium rate,
And being sequentially increased with ball milling oxalic acid amount illustrates that the modification of different oxalic acid is attained by the height of chromium except chromium rate is sequentially increased
Effect removal.
3 ball milling oxalic acid Zero-valent Iron pollution administration Mercury in Water Body effect picture of embodiment
5.6g Zero-valent Iron (partial size is up to 80 μm) and 0.126g oxalic acid (containing two water) are put into ball grinder, revolving speed is
550r/min, Ball-milling Time 2h, washing alcohol wash vacuum drying and obtain oxalic acid Zero-valent Iron, i.e. Fe/Ox (n=1.0%).Use mercury
The mercuric chloride solution 30mL that concentration is 5mg/L simulates mercury waste water, and pH value of solution 7.0, temperature is 25 DEG C, and Fe/Ox sample is added
0.1g, is put into the shaking table that revolving speed is 150r/min, periodically samples, and surveys mercury in solution with inductive coupling plasma emission spectrograph
Concentration, while using non-oxalic acid Zero-valent Iron as control experiment, as a result see Fig. 4.Non- oxalic acid Zero-valent Iron is slowly gone in 120min
The removal of mercury, and oxalic acid Zero-valent Iron has completely removed mercury in 10min.Illustrate that oxalic acid Zero-valent Iron can reach efficiently going for mercury
It removes.
Silver-colored effect picture in 4 ball milling oxalic acid Zero-valent Iron pollution administration water body of embodiment
5.6g Zero-valent Iron (partial size is up to 40 μm) and 0.126g oxalic acid (containing two water) are put into ball grinder, revolving speed is
550r/min, Ball-milling Time 2h, washing alcohol wash vacuum drying and obtain oxalic acid Zero-valent Iron, i.e. Fe/Ox (n=1.0%).With silver
The silver nitrate solution 30mL that concentration is 5mg/L simulates silver waste water, and pH value of solution 6.5, temperature is 25 DEG C, and Fe/Ox sample is added
0.1g is put into the shaking table that revolving speed is 150r/min, periodically samples, surveys silver concentration in solution, while being with non-oxalic acid Zero-valent Iron
As a result Fig. 5 is shown in control experiment.Non- oxalic acid Zero-valent Iron can slowly go desilver in 120min, and oxalic acid Zero-valent Iron exists
Silver has been completely removed in 10min.Illustrate that oxalic acid Zero-valent Iron can reach the efficient removal of silver.
Lead effect picture in 5 ball milling oxalic acid Zero-valent Iron pollution administration water body of embodiment
5.6g Zero-valent Iron (partial size is up to 80 μm) and 0.126g oxalic acid (containing two water) are put into ball grinder, revolving speed is
550r/min, Ball-milling Time 1h, washing alcohol wash vacuum drying and obtain oxalic acid Zero-valent Iron, i.e. Fe/Ox (n=1.0%).Use lead
The lead nitrate solution 30mL that concentration is 10mg/L simulates lead waste water, and pH value of solution 6.5, temperature is 25 DEG C, and Fe/Ox sample is added
0.1g is put into the shaking table that revolving speed is 150r/min, periodically samples, surveys lead concentration in solution, while being with non-oxalic acid Zero-valent Iron
As a result Fig. 6 is shown in control experiment.The rate constant of oxalic acid Zero-valent Iron removal lead is 2 times of non-oxalic acid Zero-valent Iron, illustrates oxalic acid
The efficient removal of lead can be reached by changing Zero-valent Iron.
Nickel effect picture in 6 ball milling oxalic acid Zero-valent Iron pollution administration water body of embodiment
5.6g Zero-valent Iron (partial size is up to 160 μm) and 0.252g oxalic acid (containing two water) are put into ball grinder, revolving speed is
800r/min, Ball-milling Time 4h, sample wash vacuum drying through washing alcohol and obtain oxalic acid Zero-valent Iron, i.e. Fe/Ox (n=
2.0%).Nickel waste water is simulated with the nickel chloride solution 50mL that nickel concentration is 20mg/L, Fe/Ox sample is added in pH value of solution 8
0.05g is put into the shaking table that revolving speed is 400r/min, 10 DEG C of temperature, periodically samples, survey in solution and remain nickel concentration, while with not
Oxalic acid Zero-valent Iron is control experiment, as a result sees Fig. 7.Oxalic acid Zero-valent Iron eliminates 98% in 40min, and non-oxalic acidization zero
Valence iron only eliminates 60% in 90min, illustrates that oxalic acid Zero-valent Iron can reach the efficient removal of nickel.
Claims (10)
1. a kind of method based on the efficient heavy-metal ion removal of ball milling oxalic acid Zero-valent Iron, it is characterised in that：By ball milling oxalic acid
Change Zero-valent Iron to be added in the aqueous solution containing heavy metal ion, carries out the removal of heavy metal ion, the ball milling oxalic acidization zero
Valence iron is that oxalic acid and Zero-valent Iron are prepared by solid-phase ball milling method.
2. according to the method described in claim 1, it is characterized in that：Through washing after the oxalic acid and Zero-valent Iron ball milling, vacuum is dry
It is dry to obtain oxalic acid Zero-valent Iron.
3. according to the method described in claim 1, it is characterized in that：The molar percentage that the oxalic acid accounts for Zero-valent Iron is：
0.2-2.0%.
4. according to the method described in claim 1, it is characterized in that：The Ball-milling Time：0.5-5h, rotational speed of ball-mill 300-
800r/min。
5. according to the method described in claim 1, it is characterized in that：Partial size, pattern, purity and the resting period of the Zero-valent Iron
No requirement (NR).
6. according to the method described in claim 1, it is characterized in that：The oxalic acid purity is technical grade or more.
7. according to the method described in claim 1, it is characterized in that：The dosage of the ball milling oxalic acid Zero-valent Iron is 1-5g/
L。
8. according to the method described in claim 1, it is characterized in that：The concentration of heavy metal ion is 2-50ppm, reaction temperature
Degree is 10-30 DEG C, and reaction pH is 4-8.
9. according to the method described in claim 1, it is characterized in that：Shaken in removal process with shaking table, make heavy metal ion and
Zero-valent Iron comes into full contact with.
10. according to the method described in claim 1, it is characterized in that：The heavy metal includes but is not limited to chromium, and mercury is silver-colored,
Lead, nickel.
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Cited By (14)
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| CN110201992A (en) * | 2019-05-16 | 2019-09-06 | 常熟理工学院 | A kind of detoxification of chromium-polluted soil |
| CN110606538A (en) * | 2019-07-30 | 2019-12-24 | 华中师范大学 | Method for removing pollutants based on efficient reduction of borated zero-valent iron |
| CN110713242A (en) * | 2019-08-09 | 2020-01-21 | 中国科学院地理科学与资源研究所 | Zero-valent iron material Fe @ iron fluoride and preparation method thereof |
| CN112062259A (en) * | 2020-09-23 | 2020-12-11 | 中国环境科学研究院 | Method for degrading organic pollutants by using interface-targeted activated persulfate |
| CN112079417A (en) * | 2020-09-23 | 2020-12-15 | 华中师范大学 | Surface humation zero-valent iron and preparation method and application thereof |
| CN112139508A (en) * | 2020-09-23 | 2020-12-29 | 中国科学院地理科学与资源研究所 | Amphoteric surface micron zero-valent iron, and preparation method and application thereof |
| CN112250156A (en) * | 2020-10-16 | 2021-01-22 | 中国环境科学研究院 | Silicification modified zero-valent iron and preparation method and application thereof |
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| US20220118516A1 (en) * | 2020-10-16 | 2022-04-21 | Chinese Research Academy Of Environmental Sciences | Silicified modified zero-valent iron and its preparation method and application |
| CN115159598A (en) * | 2022-07-27 | 2022-10-11 | 湖北省生态环境科学研究院(省生态环境工程评估中心) | Preparation method and application of sodium oxalate doped modified nano zero-valent iron |
| CN115403124A (en) * | 2022-09-09 | 2022-11-29 | 浙江工业大学绍兴研究院 | Method for efficiently removing heavy metal pollutants by ball milling of sargassum acidized zero-valent iron composite material |
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| CN115583712A (en) * | 2022-11-09 | 2023-01-10 | 华中师范大学 | Method for removing halohydrocarbon and heavy metal composite pollutants in water body by oxalic acid modified zero-valent iron and hydrotalcite physical mixture |
| CN117509847A (en) * | 2023-11-09 | 2024-02-06 | 华中师范大学 | Method for removing water bacteria and antibiotic resistance genes of copper ion coupled zero-valent iron |
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| CN110606538A (en) * | 2019-07-30 | 2019-12-24 | 华中师范大学 | Method for removing pollutants based on efficient reduction of borated zero-valent iron |
| CN110713242A (en) * | 2019-08-09 | 2020-01-21 | 中国科学院地理科学与资源研究所 | Zero-valent iron material Fe @ iron fluoride and preparation method thereof |
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| US20220118516A1 (en) * | 2020-10-16 | 2022-04-21 | Chinese Research Academy Of Environmental Sciences | Silicified modified zero-valent iron and its preparation method and application |
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| CN114291992A (en) * | 2021-12-29 | 2022-04-08 | 华中师范大学 | Preparation combination for removing municipal sludge antibiotic resistance genes and application |
| CN115159598A (en) * | 2022-07-27 | 2022-10-11 | 湖北省生态环境科学研究院(省生态环境工程评估中心) | Preparation method and application of sodium oxalate doped modified nano zero-valent iron |
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