CN106179204A - A kind of novel mercapto graphene oxide/iron and manganese oxides composite for removing methyl mercury in water body and preparation method - Google Patents
A kind of novel mercapto graphene oxide/iron and manganese oxides composite for removing methyl mercury in water body and preparation method Download PDFInfo
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- CN106179204A CN106179204A CN201610531964.8A CN201610531964A CN106179204A CN 106179204 A CN106179204 A CN 106179204A CN 201610531964 A CN201610531964 A CN 201610531964A CN 106179204 A CN106179204 A CN 106179204A
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- graphene oxide
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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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
- B01J20/28057—Surface area, e.g. B.E.T specific surface area
- B01J20/28061—Surface area, e.g. B.E.T specific surface area being in the range 100-500 m2/g
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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
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
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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
Abstract
The preparation method of novel mercapto graphene oxide/iron and manganese oxides composite is easy, its step includes: be sequentially added into ferrous sulfate and potassium permanganate solution in graphene oxide suspension, mixing and adjust pH is 7.5, stirring, stand, it is washed to neutrality, after lyophilization, obtains graphene oxide/iron and manganese oxides composite powder.With the above-mentioned powder of ethanol purge, ultrasonic disperse 1 hour in toluene, it is dispersed in after ethanol purge in 2%3 mercaptopropyi trimethoxy silanes (95% ethanol) solution and stirs 6 hours, being adjusted to pH with ammonia be 9.5 and stir 24 hours, washing lyophilization obtain sulfhydrylation graphene oxide/iron and manganese oxides composite powder.Graphene oxide is combined with iron and manganese oxides, prevents the reunion of Fe-Mn oxidation composition granule, and the introducing of sulfydryl significantly improves the removal effect of methyl mercury in water.The present invention has the advantages such as technique is simple, effect stability, applied widely, environmental friendliness, selectivity are strong.
Description
Technical field
The invention belongs to water-treatment technology field, relate to a kind of novel mercaptoization oxidation for removing methyl mercury in water body
Graphene/iron and manganese oxides composite and preparation method thereof.
Background technology
Methyl mercury is the organic neurotoxin of metal (mercury shape that toxicity is the strongest) that a kind of toxicity is extremely strong, generally through sulfate
Reducing bacteria is under anoxic conditions by Hg2+Methylate formation, owing to it persistently exists in body and can pass through food chain biology
The mankind and wild animals and plants health are threatened by enrichment.Methyl mercury to brain injury greatly, especially to control motor skill,
The nervous system of language and memory causes damage.Methyl mercury formation, migration and biological accumulation in water body and soil is complete
The environmental problem that the world pays close attention to jointly, World Health Organization (WHO) and EPA intake the highest to human body methyl mercury limits respectively
For 1.6 μ g/kg weekly and μ g/kg every day 0.1.
Removal technical research to methyl mercury is little in the world, mainly includes light degradation, biodegradation, flocculates and adsorb.
Wherein, adsorption technology is due to low cost, simple to operate, effective it is considered to be a kind of very promising technology.But, it is used for
Remove methyl mercury adsorbent report and few, mainly include biological adsorption agent (such as, Herba Spirodelae, Herba Coriandri, western paddy rice residue),
Chitosan-phospholipid complex (such as, barbital/chitosan crosslinked thing), and metal oxide composite (such as, the hydrogen of ferrum
Oxide, the polymer of divinylbenzene/ferroso-ferric oxide).Above adsorbent there is also a lot of shortcoming, such as, mechanical strength is low,
The chemical bond that poor selectivity is combined with methyl mercury is more weak, the degradation under removal efficiency when the concentration of methyl mercury is relatively low.
Graphene oxide, as the nano material got most of the attention in recent years, has mono-layer graphite structure, huge theory ratio
Surface area, high mechanical properties and abundant functional group, can be by cheap graphite powder batch production, and the character of these uniquenesses makes
Graphene oxide and composite having a extensive future in environmental pollution reparation thereof.
Sulfydryl (-SH) easily with mercury atom combine, graphene oxide that modified with mercapto group is crossed and composite counterweight thereof
Mercury metal shows higher absorption property.Such as, through the graphene oxide/ferriferrous oxide composite material of sulfhydrylation to Hg2+
Deng maximum adsorption capacity (Qmax) up to 289.9mg/g (during without sulfhydrylation, QmaxIt is only 16.60mg/g).Document
" A.S.Krishna Kumar, S.-J.Jiang, W.-L.Tseng, Facile synthesis and
characterization of thiol-functionalized graphene oxide as effective
Adsorbent for Hg (II), J.Environ.Chem.Eng.4 (2016) 2052-2065. " report sulfhydrylation oxidation stone
Ink alkene, when pH ≈ 7, is 98% to the methyl mercury clearance that initial concentration is 30mg/L, maximum adsorption capacity (Qmax) up to
48.07mg/g, this institute methyl mercury excessive concentration, differ greatly with actual environment concentration, therefore, it is necessary to develop one
Both there is high absorption capacity, Low Level Methylmercury had been had the environmentally friendly adsorbent of good removal effect simultaneously.
Research finds, graphene oxide/iron and manganese oxides has the big (153m of specific surface area2/ g), higher inorganic mercury (Hg2 +) adsorption capacity (Qmax=32.90mg/g), the feature such as preparation is simple, be easily isolated, it is possible to decrease hydrargyrum is to Semen Tritici aestivi and the biology of Oryza sativa L.
Toxicity, repairs field at water body and heavy metal pollution of soil and has broad application prospects, but this material is to methyl mercury adsorption effect
The best, this material sulfhydrylation is expected to improve the removal to methyl mercury, but pertinent literature is not reported.
Summary of the invention
Novel mercapto graphene oxide/iron and manganese oxides composite the most of the present invention, be by graphene oxide/
Iron and manganese oxides synthesizes through 3-mercaptopropyi trimethoxy silane sulfhydrylation, it is characterised in that: described 3-mercaptopropyi trimethoxy
Base silane hydrolyzes under conditions of ammonia exists, and by the oxygen-containing functional group with graphene oxide/iron and manganese oxides surface (i.e.
C=O, C-O-C, O=C-O, C-O) and the effect of pi-pi bond combine.
Novel mercapto graphene oxide/iron and manganese oxides composite the most of the present invention, it is characterised in that: described
Sulfhydrylation graphene oxide/iron and manganese oxides composite is in preparation process, and the mol ratio of ferrum and manganese is 3/1, ferrum and oxidation
The mass ratio of Graphene is 1/7.5, and the concentration of volume percent of 3-mercaptopropyi trimethoxy silane and ethanol is respectively 2% He
95%.
Novel mercapto graphene oxide/iron and manganese oxides composite the most of the present invention, it is characterised in that: preparation
Step is easy.
The preparation of novel mercapto graphene oxide/iron and manganese oxides composite: in graphene oxide suspension successively
Adding ferrous sulfate and potassium permanganate solution, mixing and adjust pH is 7.5, stirring, stands, is washed to neutrality, obtains after drying
Graphene oxide/iron and manganese oxides composite powder.Graphene oxide/iron and manganese oxides the powder prepared with ethanol purge
3 times, ultrasonic disperse 1 hour in toluene subsequently, after ethanol purge 3 times, it is dispersed in 2%3-mercaptopropyi trimethoxy silane
In (95% ethanol) solution and stir 6 hours, being adjusted to pH with ammonia subsequently and be 9.5 and stir 24 hours, last centrifugation obtains
To solid material and be washed to neutrality, freeze-dried obtain sulfhydrylation graphene oxide/iron and manganese oxides composite powder.
Novel mercapto graphene oxide/iron and manganese oxides composite the most of the present invention, it is characterised in that to water
Methyl mercury removal effect in body is notable.When methyl mercury initial concentration is 50 μ/L, material dosage be 50mg/L, pH=7.0 ±
0.2, ionic strength is 0.01M NaNO3Time, after mixing 24h, the clearance of methyl mercury is 91%, and clearance is under the same terms
9.8 times (methyl mercury clearance is only 9.3%) without the graphene oxide/iron and manganese oxides of sulfhydrylation.
Atomic fluorescence used by the detection of methyl mercury the most of the present invention (Ji Tian AFS-830) testing conditions is as follows: negative height
Pressure: 270V；Atomizer height: 8mm；Lamp current: 30mA；Carrier gas flux: 300mL/min；Shield gas flow amount: 800mL/min.
Detailed description of the invention:
It is further elucidated with the present invention in conjunction with case study on implementation in detail below.It should be understood that implementation below is only used for explaining this
Invention, and it is not intended to the scope of application of the present invention.The experimental technique of unreceipted actual conditions in following embodiments, generally according to
Normal condition operates.
Embodiment:
This enforcement provides the preparation side of the novel mercapto graphene oxide/iron and manganese oxides composite of a kind of simplicity
Method, and it is applied to the absorption of methyl mercury in water body.The system of novel mercapto graphene oxide/iron and manganese oxides composite
Standby operation is simple: (Mn/Fe mol ratio is to be sequentially added into ferrous sulfate and potassium permanganate solution in graphene oxide suspension
0.33, Fe/GO mass ratio is 1/7.5), mixing and adjust pH is 7.5, stirring, stands, is washed to neutrality, after lyophilization
To graphene oxide/iron and manganese oxides composite powder.Weigh 150mg graphene oxide/iron and manganese oxides powder, use ethanol
Clean 3 times (200mL), ultrasonic (300W) in toluene (30mL) subsequently disperse 1 hour, divide after ethanol purge 3 times (200mL)
It is dispersed in 300mL 2%3-mercaptopropyi trimethoxy silane (95% ethanol) solution and stirs 6 hours, being adjusted to ammonia subsequently
PH is 9.5 and continuously stirred 24 hours, is finally centrifugally separating to obtain solid material and washes 5 times (300mL), lyophilization (-60
DEG C, 48h) obtain powder sulfhydrylation graphene oxide/iron and manganese oxides composite, it is labeled as GFMSH.Graphene oxide/
Iron and manganese oxides is labeled as GFM.
Observing composite material surface form by transmission electron microscope (TEM), result is as it is shown in figure 1, iron and manganese oxides
Particle height is dispersed in surface of graphene oxide, and iron and manganese oxides particle size is less than 10nm.
By contrast graphene oxide (GO), graphene oxide/iron and manganese oxides (GFM) and sulfhydrylation graphene oxide/
The Fourier transform infrared spectroscopy (FTIR) of iron and manganese oxides (GFMSH), research surface functional group kind change.Result such as Fig. 2
Shown in, in the spectrogram of GFMSH, 679,900, and 1105cm-1It it is the stretching vibration of C-S, Si-O, and Si-C, it is seen that 3-sulfydryl
Propyl trimethoxy silicane is successfully supported on GFM surface, and S-H is at 2600-2550cm-1There is a more weak stretching vibration at place,
Due to usually by CO2Shattering zone covers and is difficult to detect by.3408,1716,1401,1243,1047 and 1621cm-1It is-OH,
C=O, O=C-O/C-OH, C-O-C, C-O and sp2C=C stretching vibration, it is seen that the oxygen-containing functional group in GO depends in GFMSH
So exist, and above-mentioned functional group peak intensity in GFMSH strengthen, illustrate 3-mercaptopropyi trimethoxy silane by with GFM
The oxygen-containing functional group (i.e. C=O, C-O-C, O=C-O, C-O) on surface is connected with the effect of pi-pi bond, and GFMSH is in adsorption process
In there is more active site position.
Raman spectrum result such as Fig. 3, the peak intensity ratio I of two peak bands (D band and G carry)D/IGSize order is: 0.872
(GFMSH) ＞ 0.817 (GFM) ＞ 0.801 (GO), illustrates that the carbon structure in GFMSH exists more defect than GFM and GO, knot
Opinion is consistent with infrared spectrum.
In order to contrast GFM and GFMSH to the removal effect of Low Level Methylmercury in water body, individually add two kinds of absorption
Agent carries out methyl mercury adsorption experiment.Sample is placed in 30mL politef (PTFE) bottle, and at room temperature (25 DEG C) use and rotate
Incubator (40rpm) turn upside down rotation 72h, all experimental grouies and matched group be all provided with 3 groups parallel.After having tested, use
Low speed centrifuge 5000rpm is centrifuged 10min, takes supernatant respectively and measures the residual concentration of wherein methyl mercury.All experiment conditions
Keep consistent, it may be assumed that methyl mercury initial concentration is 50 μ g/L, and adsorbent dosage is 50mg/L, pH=7.0 ± 0.2, ionic strength
For 0.01M NaNO3, reaction system is 28mL, and the response time is 72h.Experimental result as shown in Figure 4, after reacting 24 hours,
GFMSH is 91% to the clearance of methyl mercury, for 9.8 times (clearances 9.3%) of GFM without sulfhydrylation under the same terms,
Illustrate this material sulfhydrylation can be significantly improved the absorbability to methyl mercury.
The detection method of hydrargyrum according to People's Republic of China's state environment protecting standard (HJ694-2014) " water quality-hydrargyrum,
Mensuration-the atomic fluorescence method of arsenic, selenium, bismuth and antimony " detect.Atomic fluorescence (Ji Tian AFS-830) testing conditions used is as follows:
Negative high voltage: 270V；Atomizer height: 8mm；Lamp current: 30mA；Carrier gas flux: 300mL/min；Shield gas flow amount: 800mL/
min。
In order to investigate GFMSH to the absorption property of methyl mercury and the adsorption effect under different methyl mercury initial concentrations,
Adsorption dynamics adsorption kinetics and adsorption isotherm experiment are carried out.Dynamic experiment condition: methyl mercury initial concentration is 50 μ g/L, adsorbent
Dosage is 50mg/L, pH=7.0 ± 0.2, and ionic strength is 0.01M NaNO3, reaction system is 28mL, and the response time is
72h.Adsorption isotherm experiment condition: methyl mercury initial concentration is 50-900 μ g/L, and remaining condition is ibid.Experimental result such as Fig. 5 institute
Show.Fig. 5 A is the GFMSH clearance versus time curve to methyl mercury, and visible in figure, clearance reaches rapidly in 1.5h
To 76.8%, the most slowly raising, within the 3rd day, clearance is stable 91%, second-order kinetic equation (R2=0.999, Fig. 5 C) ratio
First _ order kinetics equation (R2=0.717, Fig. 5 B) more preferable this adsorption process of matching.Adsorption isotherm experimental result (Fig. 5 D)
Show, Langmuir model (R2=0.992) and Freundlich (R2=0.996) model all energy well matching experimental data,
Methyl mercury maximum adsorption capacity (Qmax) up to 47.16mg/g.
In general, sulfhydrylation graphene oxide/iron and manganese oxides composite have advantages of good adsorption effect, selectivity strong,
Preparation is simple, adsorption capacity advantages of higher, is with a wide range of applications in terms of heavy metal-polluted water reparation.
Accompanying drawing illustrates:
Fig. 1 is the transmission electron microscope figure of sulfhydrylation graphene oxide/iron and manganese oxides (GFMSH)；
Fig. 2 is graphene oxide (GO), graphene oxide/iron and manganese oxides (GFM), sulfhydrylation graphene oxide/ferrimanganic
The FTIR spectrum figure of oxide (GFMSH)；
Fig. 3 is graphene oxide (GO), graphene oxide/iron and manganese oxides (GFM), sulfhydrylation graphene oxide/ferrimanganic
The Raman spectrogram of oxide (GFMSH)；
Fig. 4 is graphene oxide/iron and manganese oxides (GFM) and sulfhydrylation graphene oxide/Fe-Mn oxidation under the same terms
The thing (GFMSH) the removal effect figure to methyl mercury；
Fig. 5 is sulfhydrylation graphene oxide/iron and manganese oxides (GFMSH) to the adsorption dynamics adsorption kinetics of methyl mercury and adsorption isotherm
Line chart.
Claims (5)
1. novel mercapto graphene oxide/iron and manganese oxides composite and the preparation being used for removing methyl mercury in water body
Method, it is characterised in that iron and manganese oxides is highly dispersed in surface of graphene oxide, and 3-mercaptopropyi trimethoxy silane is at ammonia
Hydrolysis oxygen-containing functional group (i.e. C=O, C-O-C, O=C-O, C-with graphene oxide/iron and manganese oxides surface in the presence of water
O) it is connected with the effect of pi-pi bond.
Novel mercapto graphene oxide/iron and manganese oxides composite the most according to claim 1, it is characterised in that:
Described sulfhydrylation graphene oxide/iron and manganese oxides composite is during preparation, and the mol ratio of ferrum and manganese is 3: 1, ferrum
Being 1: 7.5 with the mass ratio of graphene oxide, the concentration of volume percent of 3-mercaptopropyi trimethoxy silane and ethanol is respectively
It is 2% and 95%.
3. according to the novel mercapto graphene oxide/iron and manganese oxides composite described in claim 1 to 2, its feature
It is that preparation process is easy.
The preparation of novel mercapto graphene oxide/iron and manganese oxides composite: be sequentially added in graphene oxide suspension
Ferrous sulfate and potassium permanganate solution, mixing and adjust pH is 7.5, stirring, stands, is washed to neutrality, obtains after lyophilization
Graphene oxide/iron and manganese oxides composite powder.Graphene oxide/iron and manganese oxides the powder prepared with ethanol purge
3 times, ultrasonic disperse 1 hour in toluene subsequently, after ethanol purge 3 times, it is dispersed in 2%3-mercaptopropyi trimethoxy silane
In (95% ethanol) solution and stir 6 hours, being adjusted to pH with ammonia subsequently and be 9.5 and stir 24 hours, last centrifugation obtains
To solid material and be washed to neutrality, lyophilization obtains sulfhydrylation graphene oxide/iron and manganese oxides composite powder.
4. the novel mercapto graphene oxide/iron and manganese oxides composite described in claims 1 to 3, it is characterised in that can
Efficiently removing the methyl mercury of low concentration in water body, removal effect is better than similar adsorbent.
5. the detection method of the methyl mercury described in claim 4 is according to People's Republic of China's state environment protecting standard
(HJ694-2014) " mensuration-atomic fluorescence method of water quality-hydrargyrum, arsenic, selenium, bismuth and antimony " detects.Reduction used by the method
Methyl mercury Restore All can be nonvalent mercury by agent potassium borohydride, and atomic fluorescence used (Ji Tian AFS-830) testing conditions is as follows:
Negative high voltage: 270V；Atomizer height: 8mm；Lamp current: 30mA；Carrier gas flux: 300mL/min；Shield gas flow amount: 800mL/
min。
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Cited By (6)
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| CN106861646A (en) * | 2017-04-01 | 2017-06-20 | 东华大学 | The preparation method of the sorbing material of selective absorption silver ion |
| CN109607525A (en) * | 2019-01-15 | 2019-04-12 | 哈尔滨工业大学 | A kind of preparation method and application for the graphene oxide composite material that fold is mercapto-functionalized |
| CN109772271A (en) * | 2019-03-14 | 2019-05-21 | 中国科学院生态环境研究中心 | Modified algae adsorbent of a kind of ferrimanganic and preparation method thereof |
| CN109837093A (en) * | 2019-03-01 | 2019-06-04 | 中科京投环境科技江苏有限公司 | The restorative procedure of mercury contaminated soil |
| CN111847625A (en) * | 2020-07-17 | 2020-10-30 | 吉林大学 | Method and device for removing methyl mercury in sewage by using ternary composite nano material |
| CN114314798A (en) * | 2021-12-30 | 2022-04-12 | 华夏碧水环保科技有限公司 | Method for removing organic pollutants by activating persulfate through diatomite composite loaded with iron and manganese |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106861646A (en) * | 2017-04-01 | 2017-06-20 | 东华大学 | The preparation method of the sorbing material of selective absorption silver ion |
| CN106861646B (en) * | 2017-04-01 | 2019-05-07 | 东华大学 | The preparation method of the adsorbent material of selective absorption silver ion |
| CN109607525A (en) * | 2019-01-15 | 2019-04-12 | 哈尔滨工业大学 | A kind of preparation method and application for the graphene oxide composite material that fold is mercapto-functionalized |
| CN109837093A (en) * | 2019-03-01 | 2019-06-04 | 中科京投环境科技江苏有限公司 | The restorative procedure of mercury contaminated soil |
| CN109772271A (en) * | 2019-03-14 | 2019-05-21 | 中国科学院生态环境研究中心 | Modified algae adsorbent of a kind of ferrimanganic and preparation method thereof |
| CN111847625A (en) * | 2020-07-17 | 2020-10-30 | 吉林大学 | Method and device for removing methyl mercury in sewage by using ternary composite nano material |
| CN111847625B (en) * | 2020-07-17 | 2023-01-31 | 吉林大学 | Method and device for removing methyl mercury in sewage by using ternary composite nano material |
| CN114314798A (en) * | 2021-12-30 | 2022-04-12 | 华夏碧水环保科技有限公司 | Method for removing organic pollutants by activating persulfate through diatomite composite loaded with iron and manganese |
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Application publication date: 20161207 |