CN105945299A - Application of nano-iron synthesized by tea leaves in p,p'-DDT removal - Google Patents
Application of nano-iron synthesized by tea leaves in p,p'-DDT removal Download PDFInfo
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- CN105945299A CN105945299A CN201610274411.9A CN201610274411A CN105945299A CN 105945299 A CN105945299 A CN 105945299A CN 201610274411 A CN201610274411 A CN 201610274411A CN 105945299 A CN105945299 A CN 105945299A
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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
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09C—RECLAMATION OF CONTAMINATED SOIL
- B09C1/00—Reclamation of contaminated soil
- B09C1/08—Reclamation of contaminated soil chemically
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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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
- C02F2101/30—Organic compounds
- C02F2101/36—Organic compounds containing halogen
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Abstract
The invention discloses the application of nano-iron synthesized by tea leaves in p,p'-DDT removal. According to the application, tea powder which is located near the root and has long growth cycle is mixed with ultrapure water according to the proportion of 1g:10-40 mL, and centrifugation and filtration are conducted, so that a tea leaf extracting solution is obtained; and the tea leaf extracting solution and an FeSO4 solution with the concentration being 0.1 mol/L are mixed according to the volume ratio of 2:1, and oscillation is conducted for 30 min under the conditions that the temperature is 25 DEG C and the rotating speed is 250 rpm, so that green nano-iron turbid liquid is obtained. The application of the nano-iron synthesized by tea leaves in p,p'-DDT removal has the advantages that equipment is simple, the application can be conducted at the normal temperature and pressure, the cost is low, and environmental friendliness is achieved; and in addition, the application belongs to waste utilization, the requirements for the technical conditions are low, the time efficiency is high, and industrial production can be achieved hopefully. The p,p'-DDT degradation efficiency of the obtained nano-iron is remarkably improved, and the nano-iron has good application prospects in the field of organic pollutant degradation.
Description
Technical field
The present invention relates to the preparation method of Preen nono ferrum suspension, particularly one utilizes leaf of tea tree to close
The Nanoscale Iron become is in the application removed on p, p '-DDT.
Background technology
DDT is typical organochlorine pesticide, belongs to persistence organic pollutant.China is raw as agricultural
Producing big country, be that pesticide first consumes big country and the second big producing country in the world, wherein organochlorine pesticide is
The pesticide that China is main, its yield has exceeded the 50% of China's pesticide total amount.1970, clofenotane,
The organochlorine pesticide amount of making such as Gamma Hexaochlorocyclohexane and toxaphene reaches 19.17 ten thousand tons, and its value has reached overall Pesticide use
About the 80% of total amount.Later, along with this classical environmental protection of Rachel Carson " silent spring "
The publication of works, people start gradually to pay close attention to the safety of this efficient pesticides of DDT.The U.S., add
Put on airs and Sweden started in 1970 to implement DDT to forbid producing and Distursement, countries in the world afterwards
Implement the most successively.At present, although DDT in China not as Pesticide use, but its still as other use
Way production and application in market or environment.Main uses has: one is to use as anti-fouling paint;Two
It is that the raw material as dicofol uses, containing DDTs in the dicofol that China market is sold
Composition accounts for more than 14%;Three is as the drug use preventing malaria, although China after calendar year 2001
No longer use it for preventing and treating malaria, but still retain certain stock, when the natural calamity such as flood, earthquake occurs
Still Malaria outbreak can be prevented with it during evil.Studies have reported that, from 1988 to 2002 years, because using
Dicofol and flow into the DDTs in environment and just have about 8770 tons.Due to DDT difficult degradation, and
It is high lipophilic fat hydrophobic organic pollutant, and the crops in soil media can absorb and accumulation dirt
Dye, is then transmitted step by step by food chain and is enriched with, and finally constitutes tight to ecological environment and health
The harm of weight.
In soil, the common restorative procedure of organochlorine contamination includes that peripheral doses, chemical redemption and biology are repaiied
Multiple.Common physical method mainly includes digging, soil removal and replacement/soil moved in improve the original, ventilate, burn, thermal desorption, gas
The means such as phase extraction process and microwave extraction method.Thermal desorption technology refers under the mode of directly or indirectly heating,
When being generally heated to 150-540 DEG C, the pollutant in soil can evaporate and be recovered to be located again
Manage thus realize the reparation to contaminated soil, prevent atmosphere pollution simultaneously.This method have the process cycle short,
The advantages such as efficiency height, low cost, flexible operation, therefore become developed country to organic polluted soil reparation
One of important technology.But this technology is only suitable for the process of volatilization and half volatile pollutants, and
Thermal desorption equipment investment is bigger.Low cost needed for gas phase extraction process, easily operates, and does not destroy soil knot
Structure and do not cause the advantages such as secondary pollution, but be suitable only for processing volatility preferably, pollution scale less
Pollutant, and the later stage removal effect of pollutant is undesirable.
The chemical redemption of contaminated soil is broadly divided into two big classes: one is to add chemical redemption examination in soil
Agent so that it is certain chemical reaction occurs with pollutant, thus pollutant be degraded be converted into low toxicity or
Nontoxic compound;Two be in soil addition chemical removal reagent, its dissolubility in soil and
Mobility will be improved, so that what pollutant were eluted out reaching clearing the pollution off from soil
Effect.Common chemical repair method includes: chemical leaching method, chemical oxidation repairing method, photocatalysis
Edman degradation Edman, electrochemical degradation method etc..But chemical leaching method usually requires that there is water source near reparation place
Or facilitating diversion, after drip washing, produced eluent also needs to process further, increases the most again
Rehabilitation cost, and the long processing period of soil washing, efficiency also ratio is relatively low, for great majority
Contaminated site is the most applicable.Though photocatalysis technology can thoroughly break ring organic pollution, and will not produce
Secondary pollution, but operating cost is high in actual applications and uses limited time, is affected by light transmission,
Light-catalyzed reaction speed is relatively low, thus have impact on its industrialization.Above method generally exists costly,
It is likely to result in secondary pollution problems.
Biological treatment mainly relies on the plant of nature, microorganism or protozoacide etc. to make in soil
Poisonous and hazardous contaminant degradation becomes CO2And H2O or resolve into nontoxic, the method for low toxicity product, has
Safety, low cost, the feature of secondary pollution will not be produced, therefore be also called environmental friendliness recovery technique.
But there is also the process problem of repairing efficiency length, later stage plant, and because organochlorine pesticide pair
There is high toxicity and accumulative in biology, constrains the feasibility that animal is repaired.
Zero-valent Iron reduction dechlorination method is a kind of metal deoxidization, and organochlorine compound has halogeno-group because of it
Roll into a ball and show high toxicity and antibiont degradation property.The eighties in 20th century, American scientist Sweeny
First being found that Zero-valent Iron can be as one effective Dehalogenation reduction agent, and Zero-valent Iron has strong reduction
The superioritys such as property, honesty are easy to get, environmental friendliness, therefore the method arouses widespread concern and grinds
Study carefully.Along with the fast development of chemical molecular science, nanoscale science and technology starts appearance, nano zero valence iron
It is found the most therewith.Nano zero valence iron, compared with common Zero-valent Iron, has specific surface area reduction big, high
The features such as activity, can inject porous media and can migrate in multimedium.Additionally, nano material
Also have absorption, be catalyzed, the new features such as absorption, therefore the removal effect for organochlorine contamination is more preferable.
With common material ratio, owing to nano level material significantly improves its surface area, therefore have only to make
Just can reach identical effect with a small amount of material, raw material and energy are saved the most significantly
Cost.Up to the present, nano zero valence iron has been obtained for quickly developing, and it is by widely
It is applied to process organic and inorganic pollution in soil and water, mainly has halogenated organic compounds, multi-ring
Aromatic hydrocarbons (PAHs), pesticide, heavy metal etc., especially draw with nano zero valence iron degraded organochlorine pollutant
Play people's extensive concern.
Along with nano zero valence iron is extensively admitted, its eco-toxicity produced annoyings again research worker.
Having scholar to propose green syt method at present, green syt method is a kind of employing microorganism cultures or plant
The reductive organic matters such as the biomolecule in extracting solution such as enzyme, protein, polysaccharide, organic acid and polyphenol
The method that metal salt back is become nano metal, in building-up process, microorganism cultures or plant extract
Organic substance in liquid simultaneously works as the effect of protective agent and stabilizer.Compare with prior synthesizing method, green
Color building-up process avoids the poisonous and hazardous chemical substance of use, reduces energy expenditure, has economy
Property and the feature of environment friendly.Additionally, the mild condition needed for its reaction is controlled, yield is high, system
Default size and form is more met for the nano material gone out.Plant is just had learned that from 20 beginning of the century people
Extracting solution has the ability of reduction iron salt, although also lacking the understanding to natural reducing agent at that time.But it is true
Plant extraction liquid or plant tissue is just being utilized to carry out nano metal material synthesis the most later, in the past
The exploration of recent two decades and research, the researcher of international nanotechnology starts gradually to pay attention to green syt and receives
Rice this technology of material.
Method of the present invention utilizes leaf of tea tree to synthesize Preen nono ferrum, and is applied to p, p '-DDT's
Degraded, not only achieves the recycling of leaf of tea tree, turns waste into wealth, and the synthesis reducing Nanoscale Iron becomes
This, simultaneously synthesizing Preen nono ferrum has efficient degradation efficiency to p, p '-DDT, has widely
Application prospect.
Summary of the invention
Present invention aims to the shortcoming and defect of existing Nanoscale Iron synthetic technology, it is provided that a kind of
Utilize the Nanoscale Iron that leaf of tea tree synthesizes in the application removed on p, p '-DDT.
The preparation method of above-mentioned Preen nono ferrum comprises the following steps:
(1) tea leaf collection and process
After the leaf of tea tree washing surface impurity off is dried naturally, ground 140 mesh standard sieves, envelope
Standby.
Described leaf of tea tree be not for product drink tender leaf, and be near root, growth cycle
The longer blade without consumption value.
(2) prepared by leaf of tea tree extracting solution
By the leaf of tea tree powder that above-mentioned steps (1) obtains with ultra-pure water according to mass volume ratio it is
1:10~1:40, unit is g/mL, joins and carries out mix homogeneously in reaction vessel;It is then it is airtight,
Water bath with thermostatic control heated and stirred 1.5~3h on magnetic stirring apparatus, obtain leaf of tea tree mixed liquor;By leaf of tea tree
Mixed liquor, with under the rotating speed of 3000rpm centrifugal 5~20min, filters with organic facies filter, obtains tea
Leaves extracting solution.
(3) synthesis Preen nono ferrum
Weigh FeSO4·7H2The Fe of 0.1mol/L it is made into after O stirring and dissolving2+Solution.Leaf of tea tree extracts
Liquid and the FeSO of 0.1mol/L4Solution mixes (solution rapidly goes to black) with the volume ratio of 2:1,
At 25 DEG C, constant temperature oscillation 30min under the conditions of 250rpm, obtain Preen nono ferrum suspension.
The Preen nono ferrum being prepared from by said method can be used for removing p, the p '-DDT in water/soil,
Concrete application is as follows:
(1) removing P, the P '-DDT in contaminant water, detailed process is as follows:
First P, P '-DDT concentration and pH value in water source to be administered are measured, if P, P ' be-DDT
Concentration is 0.001~2mg/L, and pH value is in the range of 4.0~10.0, then throw at every 15mL water sample
Add 0.001~after 1mL Nanoscale Iron suspension, reach to remove the purpose of p, p '-DDT by concussion reaction.
If pH value in the range of 4.0~10.0, does not passes through H2SO4Or NaOH regulates its pH value.According to
Drinking water sanitary standard GB 5749-2006, clofenotane limit value is 0.001mg/L, if P, P '
< 0.001mg/L is then without administering for-DDT concentration;If P, P '-DDT concentration > 2mg/L, can
Suitably strengthen Nanoscale Iron dosage to reach optimal removal effect.
As preferably, water sample is 30 DEG C with the reaction temperature of Nanoscale Iron, and under the conditions of this, clearance is up to 83%
Above.
(2) removing P, the P '-DDT in contaminated soil, detailed process is as follows:
First p, p '-DDT in soil to be administered is measured, if p, p '-DDT concentration is 1.0~200.0
In the range of mg/kg, then every 5g soil adds 2.0~100.0mL Nanoscale Iron suspensions, rear by shake
Swing reaction and reach to remove the purpose of p, p '-DDT.According to standard of soil environment quality GB 15618-1995,
P, P '-DDT content grade III Standard is 1.0mg/kg, if P, P '-DDT concentration < 1.0mg/kg then without
Need to administer;If P, P '-DDT concentration > 200mg/kg, can dilute to reach most preferably to remove
Effect.
The present invention has that equipment is simple, can carry out at normal temperatures and pressures, low cost, eco-friendly
Advantage, and belong to twice laid, technical conditions require low, and timeliness is high, and (in aqueous solution, 2h is interior, native
Earth can reach in 24h good clearance), it is expected to carry out industrialized production.The Preen nono of synthesis
The degradation efficiency of p, p '-DDT is significantly increased by ferrum, has good answering in organic pollutant degradation field
Use prospect.
Accompanying drawing explanation
Fig. 1 is green syt Nanoscale Iron scanning electron microscope (SEM) figure.
Fig. 2 is green syt Nanoscale Iron energy spectrum analysis (EDS) figure.
Fig. 3 is transmission electron microscope (TEM) figure of green syt Nanoscale Iron.
Fig. 4 is X-ray diffraction (XRD) figure of green syt Nanoscale Iron.
Fig. 5 is thermogravimetric analysis (TGA) figure of green syt Nanoscale Iron.
Fig. 6 is FTIR spectrum (FTIR) figure of green syt Nanoscale Iron.
Fig. 7 be the present embodiment green syt Nanoscale Iron under condition of different temperatures in aqueous solution
P, p ' the clearance curve of-DDT.
Fig. 8 is the present embodiment green syt Nanoscale Iron under conditions of different dosages in aqueous solution
P, p ' the clearance curve of-DDT.
Fig. 9 is the present embodiment green syt Nanoscale Iron under conditions of different pH in aqueous solution
P, p ' the clearance curve of-DDT.
Figure 10 is the present embodiment green syt Nanoscale Iron clearance curve to p in soil, p '-DDT,
In 24h, clearance is up to 57.3%, and speed and effect are better than simple Zero-valent Iron.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is further analyzed.
This utilize leaf of tea tree to prepare Preen nono ferrum method to comprise the following steps:
(1) tea leaf collection and process
After the leaf of tea tree washing surface impurity off is dried naturally, ground 140 mesh standard sieves, envelope
Standby.
Described leaf of tea tree be not for product drink tender leaf, and be near root, growth cycle
The longer blade without consumption value.
(2) prepared by leaf of tea tree extracting solution
By the leaf of tea tree powder that above-mentioned steps (1) obtains with ultra-pure water according to mass volume ratio it is
1:10~1:40 (unit is g/mL), joins and carries out mix homogeneously in reaction vessel;It is then it is airtight,
Water bath with thermostatic control heated and stirred 1.5~3h on magnetic stirring apparatus, obtain leaf of tea tree mixed liquor;By leaf of tea tree
Mixed liquor, with under the rotating speed of 3000rpm centrifugal 5~20min, filters with organic facies filter, obtains tea
Leaves extracting solution.
(3) synthesis Preen nono ferrum
Weigh FeSO4·7H2The Fe of 0.1mol/L it is made into after O stirring and dissolving2+Solution.Leaf of tea tree extracts
Liquid and the FeSO of 0.1mol/L4Solution mixes (solution rapidly goes to black) with the ratio of 2:1,
25 DEG C, constant temperature oscillation 30min under the conditions of 250rpm, obtain Preen nono ferrum suspension.
Fig. 1 is green syt Nanoscale Iron scanning electron microscope (SEM) figure, and green syt nano iron particles is similar to
For spherical or ellipticity, its particle diameter is main all at 30-100nm;
Fig. 2 is green syt Nanoscale Iron energy spectrum analysis (EDS) figure.As seen from the figure, green syt Nanoscale Iron
EDS figure have the X-ray intensity peak of C, O, Fe, S, illustrate that nano grain surface exists Fe.
C, O element is essentially from the polyphenol in extracting solution and other molecule containing C, O;Figure exists S
Element-intensities peak, this is because selected FeSO4Tube-nursery Nanoscale Iron.Additionally, O element may
Also illustrate that the formation of particle surface (hydrogen) ferrum oxide because Folium Camelliae sinensis Nanoscale Iron be directly air-
Synthesis in water environment, so surface quickly can form ferrum oxide shell.EDS elementary analysis content is shown in
Table 1.
The EDS elementary analysis content of table 1 leaf of tea tree synthesis Nanoscale Iron
Fig. 3 is transmission electron microscope (TEM) figure of green syt Nanoscale Iron.This nano iron particles ratio is relatively decentralized,
Most of particle diameters are at below 100nm, but still have part Nanoscale Iron to reunite, and its particle diameter even has greatly
In 200nm;Simultaneously it is observed that this nano iron particles is spherical, this is consistent with the result of SEM;
Nano iron particles has many granules to connect into dendroid or bean chain, because carrying magnetic nano-particle
Can be by common effects such as telluric magnetic force, little intergranular magnetostatic power and surface tension.
Fig. 4 is X-ray diffraction (XRD) figure of green syt Nanoscale Iron.Leaf of tea tree green syt nanometer
Ferrum does not has obvious diffraction maximum, and this illustrates that Folium Camelliae sinensis Nanoscale Iron belongs to unbodied thing under natural environment
Matter.And it is observed that there is a faint characteristic peak at 2 θ=44~45 ° in figure, this peak is zeroth order
The absworption peak of ferrum (α-Fe).Can observe at 2 θ=25 ° scopes, have a bigger camel acromion,
This peak is from absworption peak organic in plant extraction liquid, shows that organic principle is coated with Nanoscale Iron,
Improve stability and the oxidation resistance of Nanoscale Iron, to the useful life extending green syt Nanoscale Iron
With avoiding its oxidation, there is important function.
Fig. 5 is thermogravimetric analysis (TGA) figure of green syt Nanoscale Iron.Green syt Nanoscale Iron thermal weight loss
Process is broadly divided into three phases, and the first stage is T≤170 DEG C, and leaf of tea tree Nanoscale Iron is weightless about
26.8%;Second stage is 170 DEG C, and < T≤380 DEG C, weightlessness is about 26.1%, is because Organic substance and nothing
The decomposition of setting carbon and burning;Three phases is T > 380 DEG C, and the oxide of carbon and ferrum burns completely
And generate end product Fe2O3, weightless about 16%, its quality when temperature arrives 900 DEG C is finally divided
Do not become 31.1%.
Fig. 6 is FTIR spectrum (FTIR) figure of green syt Nanoscale Iron.1426cm-1Place is tea
In leaves Nanoscale Iron, O-H deformation vibration peak in the organic acid such as tannic acid, catechuic acid, gallic acid, many
Aldehydes matter hydrolysis generates above-mentioned various organic acid, produces electronics simultaneously and is supplied to iron salt generation nanometer
Ferrum;1149cm-1Place is respectively the C-N stretching vibration peak in Nanoscale Iron fatty amine;Leaf of tea tree is received simultaneously
Meter Tie is at 525cm-1Near occur in that new absworption peak, this is Fe2O3And Fe3O4In Fe-O stretch
Contracting vibration peak.To sum up analyze, green syt nano iron particles Surface coating the polyphenol in extracting solution,
The Organic substances such as amine, carboxylic acid, ester, acyl, these Organic substances play a key effect to reducing Nanoscale Iron oxidation,
Thus improve the stability of green syt Nanoscale Iron.
Embodiment 1
(1) leaf of tea tree collection and process
The leaf of tea tree that the present invention uses all picks up from Qian Chuan town, Linan City of Zhejiang Province, and the leaf of tea tree of collection is not
The tender leaf for product drink, and be near root, the leaf without consumption value that growth cycle is longer
Sheet.After the leaf of tea tree washing surface impurity off is dried naturally, ground 140 mesh standard sieves, envelope
Standby.
(2) prepared by plant extraction liquid
10g plant powder is selected to join pyrometric cone with 200ml ultra-pure water with quality and volume ratio 1:20
Shape bottle mixes, conical flask is airtight, heating in water bath stirring 2h at 80 DEG C on magnetic stirring apparatus.
Then by plant mixed liquor with 5min centrifugal under the rotating speed of 3000rpm, the organic facies pin of 0.45 μm is crossed
Formula filter, obtains leaf of tea tree extracting solution.
(3) synthesis Preen nono ferrum
Weigh FeSO4·7H2The Fe of 0.1mol/L it is made into after O stirring and dissolving2+Solution.By 20ml plant
The 0.1mol/L FeSO of extracting solution and 10ml4Solution mixes with the ratio of 2:1 that (solution rapidly goes to black
Color), at 25 DEG C, constant temperature oscillation 30min under the conditions of 250rpm, obtain Preen nono ferrum suspension.
(4) when different reactions being set under conditions of temperature respectively 293K, 298K, 303K
Between (10min, 20min, 30min, 40min, 50min, 60min, 90min, 120min), often
Point of individual response time all does three parallel tests (relative deviation is less than 10%).It is all provided with under each temperature hierarchy
Put one group of blank experiment.
(5) pipette 100mg/L p, the p '-DDT of 0.3mL in glass centrifuge tube with liquid-transfering gun, add
Enter 10% aqueous acetone solution of 29.7mL, be configured to the DDT experimental solutions of 1mg/L.
(6) 1mL Preen nono ferrum is added by each in p, the p '-DDT solution of the 1mg/L of above-mentioned preparation
Suspension, on the offensive shake even, then with the hunting speed of 300rpm respectively at 298K, 303K, 313K
Under conditions of react.After reaction terminates, water sample is carried out pre-treatment, treats that GC-ECD detects.
In the present embodiment, green syt Nanoscale Iron temperature be 313K to aqueous solution in p, p '-DDT
Clearance reaches 76.84%.Fig. 7 be the present embodiment green syt Nanoscale Iron under condition of different temperatures to water
The clearance curve of p in solution, p '-DDT.
Embodiment 2
(1) leaf of tea tree collection and process
The leaf of tea tree that the present invention uses all picks up from Qian Chuan town, Linan City of Zhejiang Province, and the leaf of tea tree of collection is not
The tender leaf for product drink, and be near root, the leaf without consumption value that growth cycle is longer
Sheet.After the leaf of tea tree washing surface impurity off is dried naturally, ground 140 mesh standard sieves, envelope
Standby.
(2) prepared by plant extraction liquid
Plant powder is selected to join in triangular pyramidal bottle for 1:20 with quality and volume ratio with ultra-pure water
Mix, conical flask is airtight, heating in water bath stirring 2h at 80 DEG C on magnetic stirring apparatus.Then
By plant mixed liquor with 5min centrifugal under the rotating speed of 3000rpm, cross the organic facies pin type filter of 0.45 μm
Device, obtains leaf of tea tree extracting solution.
(3) synthesis Preen nono ferrum
Weigh FeSO4·7H2The Fe of 0.1mol/L it is made into after O stirring and dissolving2+Solution.Plant extraction liquid
FeSO with 0.1mol/L4Solution mixes (solution rapidly goes to black) with the ratio of 2:1,25 DEG C,
Constant temperature oscillation 30min under the conditions of 250rpm, obtains Preen nono ferrum suspension.
(4) p, the p '-DDT 0.3mL of 100mg/L is pipetted with liquid-transfering gun in the glass centrifuge tube of 50mL
In, add 10% aqueous acetone solution of 29.7mL, be configured to the p of 1mg/L, p '-DDT experimental solutions.
(5) under conditions of Preen nono ferrum suspension dosage is respectively 0.5mL, 1mL, 1.5mL
Arrange different response time (10min, 20min, 30min, 40min, 50min, 60min, 90min,
120min), point of each response time all does three parallel tests (relative deviation is less than 10%), arranges
One group of blank experiment.By 1mg/L p, the p '-DDT solution of above-mentioned preparation is separately added into 0.5mL,
The Preen nono ferrum suspension of 1mL, 1.5mL, on the offensive shake even, then with the vibration of 300rpm speed
Degree reacts under conditions of 303K.After reaction terminates, water sample is carried out pre-treatment, treats GC-ECD
Detection.
In the present embodiment, to p in aqueous solution, p '-DDT when green syt Nanoscale Iron dosage is 1.5mL
Clearance be 83.75%.Fig. 8 is the present embodiment green syt Nanoscale Iron condition at different dosages
Under clearance curve to p in aqueous solution, p '-DDT.
Embodiment 3
(1) leaf of tea tree collection and process
The leaf of tea tree that the present invention uses all picks up from Qian Chuan town, Linan City of Zhejiang Province, and the leaf of tea tree of collection is not
The tender leaf for product drink, and be near root, the leaf without consumption value that growth cycle is longer
Sheet.After the leaf of tea tree washing surface impurity off is dried naturally, ground 140 mesh standard sieves, envelope
Standby.
(2) prepared by plant extraction liquid
10g plant powder is selected to join triangle with quality and volume ratio for 1:20 with 20ml ultra-pure water
Conical flask mixes, by airtight for conical flask, heating in water bath stirring at 80 DEG C on magnetic stirring apparatus
2h.Then by plant mixed liquor with 5min centrifugal under the rotating speed of 3000rpm, the organic of 0.45 μm is crossed
Phase pin type filter, obtains leaf of tea tree extracting solution.
(3) synthesis Preen nono ferrum
Weigh FeSO4·7H2The Fe of 0.1mol/L it is made into after O stirring and dissolving2+Solution.20ml plant carries
Take the 0.1mol/L FeSO of liquid and 10ml4Solution mixes (solution rapidly goes to black) with the ratio of 2:1,
At 25 DEG C, constant temperature oscillation 30min under the conditions of 250rpm, obtain Preen nono ferrum suspension.
(4) respectively take 25mL pure acetone in 250mL volumetric flask, add ultra-pure water constant volume and be configured to 10%
Acetone, then use the H of 1mol/L2SO4Solution, the NaOH solution of 0.5mol/L and buffering
It is 2.0 that above-mentioned 10% aqueous acetone solution pH is adjusted to by liquid respectively, 3.0,4.0,5.0,6.0,7.0,8.0,
9.0, the reaction system of 11.0.Each pH point all does three parallel tests (relative deviation is less than 10%).
(5) p, the p '-DDT 0.3mL of 100mg/L is pipetted with liquid-transfering gun in the glass centrifuge tube of 50mL
In, add 10% aqueous acetone solution of 29.7mL difference pH, be configured to different pH's
1mg/Lp, p '-DDT experimental solutions.
(6) 1mL Nanoscale Iron suspension is taken in 1mg/Lp, the p '-DDT experimental solutions of above-mentioned different pH
In, on the offensive shake even, then under conditions of 303K, shake reaction with the hunting speed of 300rpm
120min.After reaction terminates, water sample is carried out pre-treatment, treats that GC-ECD detects.
In the present embodiment, green syt Nanoscale Iron when pH is 5 to aqueous solution in the going of p, p '-DDT
Except rate is 84.42%.Fig. 9 is the present embodiment green syt Nanoscale Iron under conditions of different pH to water
The clearance curve of p in solution, p '-DDT.
Embodiment 4
(1) leaf of tea tree collection and process
The leaf of tea tree that the present invention uses all picks up from Qian Chuan town, Linan City of Zhejiang Province, and the leaf of tea tree of collection is not
The tender leaf for product drink, and be near root, the leaf without consumption value that growth cycle is longer
Sheet.After the leaf of tea tree washing surface impurity off is dried naturally, ground 140 mesh standard sieves, envelope
Standby.
(2) prepared by plant extraction liquid
10g plant powder is selected to join triangle with quality and volume ratio for 1:10 with 10ml ultra-pure water
Conical flask mixes, by airtight for conical flask, heating in water bath stirring at 80 DEG C on magnetic stirring apparatus
1.5h.Then by plant mixed liquor with 20min centrifugal under the rotating speed of 3000rpm, having of 0.45 μm is crossed
Machine phase pin type filter, obtains leaf of tea tree extracting solution.
(3) synthesis Preen nono ferrum
Weigh FeSO4·7H2The Fe of 0.1mol/L it is made into after O stirring and dissolving2+Solution.20ml plant carries
Take the 0.1mol/L FeSO of liquid and 10ml4Solution mixes (solution rapidly goes to black) with the ratio of 2:1,
At 25 DEG C, constant temperature oscillation 30min under the conditions of 250rpm, obtain Preen nono ferrum suspension.
(4) pipette p, the p '-DDT of 100mg/L with liquid-transfering gun in glass centrifuge tube, add 10%
Aqueous acetone solution, is configured to 0.2mg/L DDT experimental solutions;Regulate pH to 5 the most again;
(5) 1mL nanometer is added by each in 0.2mg/L p, the p '-DDT solution of above-mentioned for 15ml preparation
Ferrum suspension, on the offensive shakes even, then carries out under the conditions of 303K with the hunting speed of 300rpm
Reaction.After reaction terminates, water sample is carried out pre-treatment, treats that GC-ECD detects.
The present embodiment green syt Nanoscale Iron reaches 87.35% to p in aqueous solution, p '-DDT clearance.
Embodiment 5
(1) leaf of tea tree collection and process
The leaf of tea tree that the present invention uses all picks up from Qian Chuan town, Linan City of Zhejiang Province, and the leaf of tea tree of collection is not
The tender leaf for product drink, and be near root, the leaf without consumption value that growth cycle is longer
Sheet.After the leaf of tea tree washing surface impurity off is dried naturally, ground 140 mesh standard sieves, envelope
Standby.
(2) prepared by plant extraction liquid
1g plant powder is selected to join triangle with quality and volume ratio for 1:40 with 40ml ultra-pure water
Conical flask mixes, by airtight for conical flask, heating in water bath stirring at 80 DEG C on magnetic stirring apparatus
3h.Then by plant mixed liquor with 10min centrifugal under the rotating speed of 3000rpm, having of 0.45 μm is crossed
Machine phase pin type filter, obtains leaf of tea tree extracting solution.
(3) synthesis Preen nono ferrum
Weigh FeSO4·7H2The Fe of 0.1mol/L it is made into after O stirring and dissolving2+Solution.20ml plant carries
Take the 0.1mol/L FeSO of liquid and 10ml4Solution mixes (solution rapidly goes to black) with the ratio of 2:1,
At 25 DEG C, constant temperature oscillation 30min under the conditions of 250rpm, obtain Preen nono ferrum suspension.
(4) pipette p, the p '-DDT of 100mg/L with liquid-transfering gun in glass centrifuge tube, add 10%
Aqueous acetone solution, is configured to 0.2mg/L DDT experimental solutions;Regulate pH to 5 the most again;
(5) by green for addition 1mL each in p, the p '-DDT solution of the 0.2mg/L of above-mentioned for 15ml preparation
Color Nanoscale Iron suspension, on the offensive shake even, then with the hunting speed of 300rpm in 303K condition
Under react.After reaction terminates, water sample is carried out pre-treatment, treats that GC-ECD detects.
The present embodiment green syt Nanoscale Iron reaches 79.22% to p in aqueous solution, p '-DDT clearance.
Embodiment 6
(1) leaf of tea tree collection and process
The leaf of tea tree that the present invention uses all picks up from Qian Chuan town, Linan City of Zhejiang Province, and the leaf of tea tree of collection is not
The tender leaf for product drink, and be near root, the leaf without consumption value that growth cycle is longer
Sheet.After the leaf of tea tree washing surface impurity off is dried naturally, ground 140 mesh standard sieves, envelope
Standby.
(2) prepared by plant extraction liquid
10g plant powder is selected to join three with quality and volume ratio for 1:30 with 300ml ultra-pure water
Mixing in pyramid bottle, conical flask is airtight, and on magnetic stirring apparatus, at 80 DEG C, heating in water bath stirs
Mix 2.5h.Then by plant mixed liquor with 5min centrifugal under the rotating speed of 3000rpm, 0.45 μm is crossed
Organic facies pin type filter, obtain leaf of tea tree extracting solution.
(3) synthesis Preen nono ferrum
Weigh FeSO4·7H2The Fe of 0.1mol/L it is made into after O stirring and dissolving2+Solution.20ml plant carries
Take the 0.1mol/L FeSO of liquid and 10ml4Solution mixes (solution rapidly goes to black) with the ratio of 2:1,
At 25 DEG C, constant temperature oscillation 30min under the conditions of 250rpm, obtain Preen nono ferrum suspension.
(4) Hangzhou insecticide factory place internal contamination soil is entered by the method that the present embodiment uses invention to propose
Row processes, and in soil, target contaminant p, p '-DDT initial concentration is 9.94mg/kg.Weighed 60 targets
Air-dried soil sample 2g of quasi-sieve, adds 2mL Preen nono ferrum suspension, puts into agitator after shaking up,
Temperature is 25 DEG C, oscillation rate is to react under conditions of 250rpm.After reaction terminates, to soil sample
Carry out pre-treatment, treat that GC-ECD detects.
The present embodiment green syt Nanoscale Iron reaches 50.2% to p in soil, p '-DDT clearance.
Embodiment 7
(1) leaf of tea tree collection and process
The leaf of tea tree that the present invention uses all picks up from Qian Chuan town, Linan City of Zhejiang Province, and the leaf of tea tree of collection is not
The tender leaf for product drink, and be near root, the leaf without consumption value that growth cycle is longer
Sheet.After the leaf of tea tree washing surface impurity off is dried naturally, ground 140 mesh standard sieves, envelope
Standby.
(2) prepared by plant extraction liquid
10g plant powder is selected to join three with quality and volume ratio for 1:20 with 200ml ultra-pure water
Mixing in pyramid bottle, conical flask is airtight, and on magnetic stirring apparatus, at 80 DEG C, heating in water bath stirs
Mix 2h.Then by plant mixed liquor with 5min centrifugal under the rotating speed of 3000rpm, having of 0.45 μm is crossed
Machine phase pin type filter, obtains leaf of tea tree extracting solution.
(3) synthesis Preen nono ferrum
Weigh FeSO4·7H2The Fe of 0.1mol/L it is made into after O stirring and dissolving2+Solution.20ml plant carries
Take the 0.1mol/LFeSO of liquid and 10ml4Solution mixes (solution rapidly goes to black) with the ratio of 2:1,
At 25 DEG C, constant temperature oscillation 30min under the conditions of 250rpm, obtain Preen nono ferrum suspension.
(4) Hangzhou insecticide factory place internal contamination soil is entered by the method that the present embodiment uses invention to propose
Row processes, and in soil, target contaminant p, p '-DDT initial concentration is 9.94mg/kg.Weighed 60 targets
Air-dried soil sample 2g of quasi-sieve, adds 2mL Preen nono ferrum suspension, arranges blank sample simultaneously and adds 2mL
Ultra-pure water, puts into agitator after shaking up, temperature be 25 DEG C, under conditions of oscillation rate is 250rpm
The different response time (2h, 4h, 6h, 8h, 10h, 24h) is set.After reaction terminates, to soil sample
Carry out pre-treatment, treat that GC-ECD detects.
Figure 10 is the present embodiment green syt Nanoscale Iron clearance curve to p in soil, p '-DDT,
Good clearance reaches 57.3%, and speed and effect are better than simple Zero-valent Iron.
Above-described embodiment is not the restriction for the present invention, and the present invention is not limited only to above-described embodiment,
As long as meeting application claims, belong to protection scope of the present invention.
Claims (5)
1. utilize Nanoscale Iron that leaf of tea tree synthesizes on a p, p '-DDT in removing polluted source
Application, it is characterised in that this Nanoscale Iron uses following steps to be prepared:
(1) tea leaf collection and process:
After the leaf of tea tree washing surface impurity off is dried naturally, ground 140 mesh standard sieves, envelope
Bag is standby;
The blade that described leaf of tea tree is near root, growth cycle is longer;
(2) prepared by leaf of tea tree extracting solution:
By the leaf of tea tree powder that above-mentioned steps (1) obtains with ultra-pure water according to mass volume ratio it is
1:10~1:40, unit is g/mL, joins and carries out mix homogeneously in reaction vessel;Then by it
Airtight, water bath with thermostatic control heated and stirred 1.5~3h on magnetic stirring apparatus, obtain leaf of tea tree mixed liquor;
By leaf of tea tree mixed liquor with under the rotating speed of 3000rpm centrifugal 5~20min, by organic facies filter mistake
Filter, obtains leaf of tea tree extracting solution;
(3) synthesis Preen nono ferrum:
Weigh FeSO4·7H2The Fe of 0.1mol/L it is made into after O stirring and dissolving2+Solution;Leaf of tea tree carries
Take the FeSO of liquid and 0.1mol/L4Solution mixes (solution rapidly goes to black) with the volume ratio of 2:1,
At 25 DEG C, constant temperature oscillation 30min under the conditions of 250rpm, obtain Preen nono ferrum suspension.
Apply the most as claimed in claim 1, it is characterised in that concrete application process is as follows:
First p, p '-DDT concentration and pH value in water source to be administered are measured, if p, p ' be-DDT
Concentration is 0.001~2mg/L, and pH value is in the range of 4.0~10.0, then at every 15mL water sample
After adding 0.001~1mL Nanoscale Iron suspension, reach to remove p, p '-DDT's by concussion reaction
Purpose;If pH value in the range of 4.0~10.0, does not passes through H2SO4Or NaOH regulates its pH
Value.
Apply the most as claimed in claim 2, it is characterised in that water sample and the reaction temperature of Nanoscale Iron
Degree is 30 DEG C.
4. utilize Nanoscale Iron that leaf of tea tree synthesizes on a p, p '-DDT in removing contaminated soil
Application, it is characterised in that this Nanoscale Iron uses following steps to be prepared:
(1) tea leaf collection and process:
After the leaf of tea tree washing surface impurity off is dried naturally, ground 140 mesh standard sieves, envelope
Bag is standby;
The blade that described leaf of tea tree is near root, growth cycle is longer;
(2) prepared by leaf of tea tree extracting solution:
By the leaf of tea tree powder that above-mentioned steps (1) obtains with ultra-pure water according to mass volume ratio it is
1:10~1:40, unit is g/mL, joins and carries out mix homogeneously in reaction vessel;Then by it
Airtight, water bath with thermostatic control heated and stirred 1.5~3h on magnetic stirring apparatus, obtain leaf of tea tree mixed liquor;
By leaf of tea tree mixed liquor with under the rotating speed of 3000rpm centrifugal 5~20min, by organic facies filter mistake
Filter, obtains leaf of tea tree extracting solution;
(3) synthesis Preen nono ferrum:
Weigh FeSO4·7H2The Fe of 0.1mol/L it is made into after O stirring and dissolving2+Solution;Leaf of tea tree carries
Take the FeSO of liquid and 0.1mol/L4Solution mixes (solution rapidly goes to black) with the volume ratio of 2:1,
At 25 DEG C, constant temperature oscillation 30min under the conditions of 250rpm, obtain Preen nono ferrum suspension.
Apply the most as claimed in claim 4, it is characterised in that concrete application process is as follows:
First p, p '-DDT in soil to be administered is measured, if p, p '-DDT concentration is 1.0~200.0
In the range of mg/kg, then every 5g soil adds 2.0~100.0mL Nanoscale Iron suspensions, after pass through
Concussion reaction reaches to remove the purpose of p, p '-DDT.
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