CN107418583A - Preparation method for the plant source heavy metal-polluted soil activator of lead-contaminated soil - Google Patents
Preparation method for the plant source heavy metal-polluted soil activator of lead-contaminated soil Download PDFInfo
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- CN107418583A CN107418583A CN201710503446.XA CN201710503446A CN107418583A CN 107418583 A CN107418583 A CN 107418583A CN 201710503446 A CN201710503446 A CN 201710503446A CN 107418583 A CN107418583 A CN 107418583A
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- C09K17/00—Soil-conditioning materials or soil-stabilising materials
- C09K17/14—Soil-conditioning materials or soil-stabilising materials containing organic compounds only
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Abstract
The present invention relates to soil conditioner field, it is desirable to provide a kind of preparation method of plant source heavy metal-polluted soil activator for lead-contaminated soil.Fresh Lemon skin obtains lemon peel slag after rubbing；Ultrapure water fraction is added thereto under agitation, is placed in after stirring together with container in reciprocating vibrating machine and carries out oscillation treatment, be then centrifuged for separating, take supernatant and filter；Chelating agent GLDA solution, biosurfactant Tea Saponin solution are added, then container is placed in reciprocating vibrating machine and carries out oscillation treatment；It is 4 to adjust the mixed liquor pH value through oscillation treatment, the closed preservation of lucifuge.The activator of the present invention, raw material sources are extensive, cheap.Preparation method is simple, takes short.It is green, secondary pollution will not be caused.
Description
Technical field
The present invention relates to soil conditioner field, especially a kind of plant source heavy metal-polluted soil for lead-contaminated soil is lived
The preparation method of agent.
Background technology
Lead is main environmental pollution element as a heavy metal species.Lead and its various form compound harm to the human body
Very big, being accumulated in human body after excess can cause lead poisoning, human respiratory, digestive system, nervous system etc. all can be by
Influence.Especially lead causes to have a strong impact on to brain functions such as the nerve of infant, cognition and memories, or even dull-witted.In recent years, due to
The use and sewage irrigation of atmospheric sedimentation, agriculture chemical film, each local soil in China is by different degrees of lead contamination, lead
Poisoning, lead content is exceeded in crop etc., and event also occurs in succession.Lead Pollution in Soil problem is increasingly severe, agricultural product security and human body
Health is by serious threat.The recovery technique of lead-contaminated soil mainly has heavy metal pollution of soil, heat treating process, electro reclamation, change at present
Fixation and elution method etc. are learned, these methods have long repair time, cost height or cause secondary pollution problems, utilize plant
Thing, which carries out plant extraction reparation, to be had the advantages that environment-friendly, non-secondary pollution and is favored by academia, but due to soil
Middle lead validity is low and influences phytoremediation efficiency, thus develop it is cheap it is efficient, environmentally friendly activator is very necessary.
Using chelating agent can activating soil heavy metal improve plant extract efficiency, chelating agent is divided into natural chelators and artificial
Two kinds of chelating agent.Wherein in the past 20 years, it is widely used for ethylenediamine tetra-acetic acid (EDTA) for the artificial synthesized chelating agent of representative
Enhancing plant extract efficiency simultaneously obtains certain effect, but EDTA is not easy to be biodegradable, and easily causes secondary pollution.Some are degradable
Green natural chelating agent such as glutamic acid N, the sodium of N- acetoacetates four (GLDA) and NTA (NTA) improve plant extract
Efficiency is increasingly becoming the focus in phytoremediation research.But these chelating agents are relatively low to the activation efficiency of lead, limit it and push away
Wide application.
Low molecular weight organic acid such as citric acid, oxalic acid etc., have the function that to activate heavy metal and environmentally friendly, can give birth to
The advantages that thing is degraded, play an important roll in heavy metal-polluted soil activation.But carry out plant using artificial synthesized organic acid
Activation extraction, not only cost is high, and its effect is influenceed by vegetation type, heavy metal species.
The content of the invention
The technical problem to be solved in the present invention is to overcome deficiency of the prior art, there is provided one kind is used to activate lead contamination
The preparation method of the heavy metallic activation agent of soil.The environmentally friendly wide material sources of heavy metallic activation agent and synthesize conveniently.
In order to solve technical problem, the technical solution adopted by the present invention is as follows：
A kind of preparation method of the plant source heavy metal-polluted soil activator for lead-contaminated soil, including following step are provided
Suddenly：
(1) Fresh Lemon skin is taken, lemon peel slag is obtained after rubbing；
(2) ultrapure water fraction time is added in lemon peel slag under agitation, the mass ratio of lemon peel slag and water is 1: 4；Stir
It is placed in after mixing uniformly together with container in reciprocating vibrating machine and carries out oscillation treatment, is then centrifuged for separating, takes supernatant and filter；
(3) chelating agent GLDA solution, biosurfactant Tea Saponin solution are added into the supernatant after filtering, then
Container is placed in reciprocating vibrating machine and carries out oscillation treatment；
The volume ratio of supernatant, GLDA solution and Tea Saponin solution is 15: 2.5: 2.5；Wherein, chelating agent GLDA solution
Mass concentration is 0.7%, and the mass concentration of Tea Saponin solution is 4%；
(4) it is 4 to adjust the mixed liquor pH value through oscillation treatment, the closed preservation of lucifuge.
In the present invention, in step (2), (3) during oscillation treatment, frequency of oscillation 250r/min, time 30min, temperature
For 20 DEG C.
In the present invention, when centrifuging in step (2), centrifuge speed 5000r/min, time 15min, temperature is
20℃。
In the present invention, the pH value of mixed liquor is adjusted using 0.1mol/L HCL solution or NaOH solution in step (4).
Inventive principle describes：
The present invention seeks that a kind of green cost of wide material sources is cheap to be used as the novel activated of main body using fruit residue
Agent, the activation to Pb in Soil can be realized, not cause environmental pollution, while realize utilization of waste as resource.
Lemon is in itself rich in the various active materials such as citric acid, total saposins and limonin, the activation efficiency of heavy metal
Significantly, and lemon peel slag as a kind of fresh squeezing remaining waste resource of lemon juice, cost is cheap and green.Tea Saponin is
Biosurfactant, and the main matter of remediating heavy metal.It can remove the weight of sour solvent and reducible state in soil
Metal, except with reduce the property such as solution surface tension, good wetability, penetrability and emulsifying dispersivity outside, when
It is also degradable during a large amount of uses in environment, preparation is easy, wide material sources, lower-price characteristic.Therefore lemon is made full use of
Lemon skin slag by Optimized Extraction Process, obtains the extract solution containing citric acid isoreactivity composition as major ingredient, by with natural chela
Assembling for mixture and biosurfactant, can both prepare new heavy metallic activation agent, can also realize the money of discarded object
Sourceization utilizes.
Heavy metal ion and content of organics polar region in ultra-pure water, play the interference and reduction for excluding heavy metal ion
Organic matter is to the chelating complexing of the ion in extraction solution, and pH is relatively stable 6.8~7.
Compared with prior art, the beneficial effects of the invention are as follows：
1st, activator of the invention, raw material sources are extensive, cheap.
2nd, preparation method of the present invention is simple, takes short.
3rd, activator of the invention is green, will not cause secondary pollution.
Brief description of the drawings
Fig. 1 is the comparison diagram of different reagent heavy metal activation efficiencies.
Block diagram is represented sequentially as in figure：Single chelating agent EDTA, lemon peel slag supernatant, lemon peel slag supernatant with
GLDA solution and Tea Saponin solution press the mixture of different volumes ratio.
Embodiment
In order that content of the present invention easily facilitates understanding, with reference to embodiment to of the present invention
Technical scheme is described further, but the present invention is not limited only to this.
It is used for the preparation method for activating the heavy metallic activation agent of lead-contaminated soil in the present invention, comprises the following steps：
(1) Fresh Lemon skin is taken, lemon peel slag is obtained after rubbing；
(2) ultrapure water fraction time is added in lemon peel slag under agitation, the mass ratio of lemon peel slag and water is 1: 4；Stir
It is placed in after mixing uniformly together with container in reciprocating vibrating machine and carries out oscillation treatment, is then centrifuged for separating, takes supernatant and filter；Shake
The frequency of oscillation for swinging processing is 250r/min, and time 30min, temperature is 20 DEG C；Centrifuge speed is 5000r/min, the time
For 15min, temperature is 20 DEG C；
(3) chelating agent GLDA solution, biosurfactant Tea Saponin solution are added into the supernatant after filtering, then
Container is placed in reciprocating vibrating machine and carries out oscillation treatment；
The volume ratio of supernatant, GLDA solution and Tea Saponin solution is 15: 2.5: 2.5；Wherein, chelating agent GLDA solution
Mass concentration is 0.7%, and the mass concentration of Tea Saponin solution is 4%；
(4) the use of 0.1mol/L mixed liquor pH value of the hydrochloric acid regulation through oscillation treatment is 4, the closed preservation of lucifuge.
Here is the concrete application example of heavy metallic activation agent：
1st, the optimum experimental condition that orthogonal experiment determines heavy metal-polluted soil activation is carried out：
When activator of the present invention is applied to the lead activation process of leaded soil, step is specifically included：Weigh soil sample about
1.000g in 50ml centrifuge tubes, take the plant source heavy metal-polluted soil activator 20ml for preparing of the present invention add corresponding to from
In heart pipe, vibration (200r/min, 12h, 25 DEG C) in vibrating machine is put into.Then by the centrifuge tube room temperature vibrated with 5000r/
Min is centrifuged 15 minutes, is taken supernatant addition 5ml concentrated nitric acids to disappear afterwards and is boiled resolution organic matter, disappears and 0.45 μm of filter membrane is crossed after boiling, utilize
ICP-OES determines solution lead concentration.
At least 9 groups of identical and equivalent soil by lead contamination are taken, every group of soil is carried out leaded with the activator of equivalent
The lead activation experiment of soil, orthogonal is carried out according to temperature, duration of oscillation and starting pH；Wherein, temperature refers to reality
Vibration temperature during middle different reagent mixing is tested, duration of oscillation refers to duration of oscillation during different reagent mixing in experiment, starting
PH refers to the pH of the mixed starting soln of activator in experiment；Experiment using 10 DEG C of vibration temperature, 20 DEG C, 30 DEG C, duration of oscillation
12h, 24h, 36h, pH 3,4,5 is originated, carry out orthogonal.After experiment terminates, Pb in Soil activation rate highest one is selected
Group, the vibration temperature of the group, duration of oscillation and starting pH are defined as optimum experimental condition；The optimum experimental condition finally determined
It it is 20 DEG C for vibration temperature, duration of oscillation 24h, starting pH is 4.
Example 1：
When carrying out the experiment using activator activating soil lead, it is necessary to determine the optimal of reagent preparation using orthogonal experiment
Vibration temperature, optimal duration of oscillation and rise optimal beginning pH, take at least 9 groups it is identical and equivalent by lead-contaminated soil, every group of soil
Pb in Soil activation experiment is carried out with identical and equivalent activator.According to the experimental result in table 1, the 5th group of soil in 9 groups of experiments
The activation rate of earth lead is up to 57.8%, and then determines that optimum experimental condition is that vibration temperature is 20 DEG C, duration of oscillation 24h,
It is 4 to originate pH.
The Orthogonal experiment results of table 1
2nd, it is determined that optimum experimental condition under, EDTA, GLDA and Tea Saponin respectively determine that at least three compares concentration value, point
Carry out not comparative experiments of the activator to lead activation effect.
a：Take at least 27 groups it is identical and equivalent by lead-contaminated soil, according to the comparison concentration value each determined, adopt respectively
It is to compare ethanedioic acid tetraacethyl (EDTA) 0.06mol/L, 0.08mol/L, 0.1mol/L of concentration value with solution concentration；Paddy ammonia
Acid, N, the mass concentration of the sodium of N- acetoacetates four (GLDA) solution is 0.5%, 0.6%, 0.7%；The quality of Tea Saponin solution is dense
Spend for 2%, 3%, the 4% Pb in Soil activation experiment for carrying out single activator, record the Pb in Soil activation rate of each group；
b：Take at least 15 groups it is identical and equivalent by lead-contaminated soil, according to the comparison concentration value each determined, adopt respectively
It is to compare the compound activator of concentration value with solution concentration, Pb in Soil activation experiment is carried out, wherein compound activator refers to：
It is 8 that lemon residue extract, which is fixed as 75%, GLDA of activator volume and Tea Saponin volume ratio,:2、6:4、5:5、4:6、2:8
Compound desorbing agent, and record each group experiment terminate after Pb in Soil activation rate；
After experiment terminates, select and compare concentration value ethanedioic acid tetraacethyl (EDTA) for 0.08mol/L, glutamic acid N, N- acetyl
The mass concentration of the sodium of acetic acid four (GLDA) is 0.7%, and the mass concentration of Tea Saponin is 4%.
3rd, the Pb in Soil activation rate after each group experiment in comparison step B terminates, selects Pb in Soil activation rate highest one
Group, the compound activator composition volume ratio and concentration of the group, as it is used for the new type compound activation for handling lead-contaminated soil
The preparation result of agent.
After experiment terminates, determine that activator is made up of lemon peel slag extract, GLDA and Tea Saponin, the extraction of lemon peel slag
The volume ratio of thing, GLDA and Tea Saponin is 15:2.5:The mass concentration of 2.5, GLDA solution is 0.7%, the matter of Tea Saponin solution
It is 4% to measure concentration.
Chelating agent GLDA used is purchased from Akzo Nobel N.V., solids content about 47%, density 1.4g/ in experiment
cm3, mean molecule quantity 351.1, wherein No. CAS is 51981-21-6.
3rd, the preparation and application of heavy metallic activation agent
Take lemon peel slag to be put into mixer, the ultra-pure water of addition averagely adds in four times, per minor tick 30s, ultra-pure water with
Lemon peel slag mass ratio is 4:1, it is uniformly mixing to obtain lemon peel slag extract.It is put into 50ml centrifuge tubes to be vibrated, at 20 DEG C
250r/min vibrates 30min.It is then placed in supercentrifuge and centrifuges, with 5000r/min high speed centrifugation 15min at 20 DEG C, it
After take supernatant to cross 0.45 μm of filter membrane.Take supernatant and GLDA solution after filtering and Tea Saponin solution by volume 15: 2.5:
2.5 mixing；Wherein, the mass concentration of chelating agent GLDA solution is 0.7%, and the mass concentration of Tea Saponin solution is 4%；Place into
In reciprocating vibrating machine, with 250r/min hunting of frequency 30min at 20 DEG C.Take mixed liquor 0.1mol/L HCL solution or
The pH of NaOH solution regulation mixed solution is 4, obtains compound activator.
Example 2：
The preparation method of heavy metal-polluted soil activator, comprises the following steps：
1) 50g lemon peel slag is taken to be put into mixer, 200g ultra-pure waters averagely add in four times, per minor tick 30s, stirring
Uniformly obtain lemon peel slag extract.
2) lemon peel slag extract is put into 50ml centrifuge tubes to be vibrated, 250r/min vibrates 30min at 20 DEG C.Then
It is put into supercentrifuge and centrifuges, 5000r/min centrifuges 15min at 20 DEG C, goes supernatant to cross 0.45 μm of filter membrane afterwards.
3) the Tea Saponin solution that supernatant and mass concentration are 0.7%GLDA solution and mass concentration 4% is taken respectively with body
Product is mixed and made into 20ml intermixtures than 15: 2.5: 2.5,15: 4: 1 and 15: 1: 4, places into reciprocating vibrating machine at 20 DEG C
24h is vibrated with 200r/min.
4) mixed liquor 0.1mol/L HCL is taken to adjust the starting pH to 4 of mixed solution.
The new soil heavy metallic activation agent made from this method handles high-concentration lead contaminated soil, activator and soil
Liquid soil than be 20:1.As a result show that gained activator is respectively 57.1%, 44.6% and to the activation rate of lead in instantiation 2
39.8%, and it can be seen from Fig. 1, single EDTA lead activation rate is 67.8%, the lead activation rate of single lemon peel slag extract
For 33.6%.Therefore, novel activated dose of the present invention while certain efficient activation efficiency is ensured, it is thus also avoided that to ring
The secondary pollution in border, and it is cheap easily prepared, reach the recycling of discarded object.
Claims (4)
- A kind of 1. preparation method of plant source heavy metal-polluted soil activator for lead-contaminated soil, it is characterised in that including with Lower step：(1) Fresh Lemon skin is taken, lemon peel slag is obtained after rubbing；(2) ultrapure water fraction time is added in lemon peel slag under agitation, the mass ratio of lemon peel slag and water is 1: 4；Stirring is equal It is placed in after even together with container in reciprocating vibrating machine and carries out oscillation treatment, be then centrifuged for separating, is taken supernatant and filter；(3) chelating agent GLDA solution, biosurfactant Tea Saponin solution are added into the supernatant after filtering, then will be held Device, which is placed in reciprocating vibrating machine, carries out oscillation treatment；The volume ratio of supernatant, GLDA solution and Tea Saponin solution is 15: 2.5: 2.5；Wherein, the quality of chelating agent GLDA solution Concentration is 0.7%, and the mass concentration of Tea Saponin solution is 4%；(4) it is 4 to adjust the mixed liquor pH value through oscillation treatment, the closed preservation of lucifuge.
- 2. according to the method for claim 1, it is characterised in that in step (2), (3) during oscillation treatment, frequency of oscillation is 250r/min, time 30min, temperature are 20 DEG C.
- 3. according to the method for claim 1, it is characterised in that when being centrifuged in step (2), centrifuge speed is 5000r/min, time 15min, temperature are 20 DEG C.
- 4. according to the method for claim 1, it is characterized in that be, in step (4) using 0.1mol/L HCL solution or NaOH solution adjusts the pH value of mixed liquor.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111250535A (en) * | 2020-02-18 | 2020-06-09 | 四川省蜀通岩土工程公司 | Heavy metal composite contaminated site soil remediation method |
| CN111499466A (en) * | 2020-03-23 | 2020-08-07 | 浙江丰瑜生态科技股份有限公司 | Slow-release soil conditioner suitable for desert soil planting and application thereof |
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| CN111250535A (en) * | 2020-02-18 | 2020-06-09 | 四川省蜀通岩土工程公司 | Heavy metal composite contaminated site soil remediation method |
| CN111499466A (en) * | 2020-03-23 | 2020-08-07 | 浙江丰瑜生态科技股份有限公司 | Slow-release soil conditioner suitable for desert soil planting and application thereof |
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