CN107418583B - Preparation method of plant-source soil heavy metal activator for lead-polluted soil - Google Patents
Preparation method of plant-source soil heavy metal activator for lead-polluted soil Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 13
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- MGFYIUFZLHCRTH-UHFFFAOYSA-N nitrilotriacetic acid Chemical compound OC(=O)CN(CC(O)=O)CC(O)=O MGFYIUFZLHCRTH-UHFFFAOYSA-N 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- 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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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
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Abstract
The invention relates to the field of soil conditioners, and aims to provide a preparation method of a plant-derived soil heavy metal activator for lead-contaminated soil. Mincing fresh lemon peel to obtain lemon peel residue; adding ultrapure water into the solution for several times under stirring, uniformly stirring, placing the solution and the container into a reciprocating shaker for shaking treatment, then performing centrifugal separation, and taking and filtering supernatant; adding a chelating agent GLDA solution and a biosurfactant tea saponin solution, and then placing the container in a reciprocating type oscillator for oscillation treatment; adjusting the pH value of the mixed solution after the oscillation treatment to be 4, and keeping the mixed solution in a dark place and in a sealed way. The activating agent of the invention has wide raw material source and low price. The preparation method is simple and short in time consumption. Green and environment-friendly, and can not cause secondary pollution.
Description
Technical Field
The invention relates to the field of soil conditioners, in particular to a preparation method of a plant source soil heavy metal activator for lead-polluted soil.
Background
Lead, as a heavy metal, is a major environmental polluting element. Lead and various compounds thereof have great harm to human bodies, lead poisoning can be caused after excessive accumulation in human bodies, and respiratory systems, digestive systems, nervous systems and the like of the human bodies are affected. Especially lead has serious influence on the brain functions of the infants, such as nerve, cognition, memory and the like, even dementia. In recent years, due to atmospheric sedimentation, the use of pesticide and fertilizer films and sewage irrigation, the soil of various places in China is polluted by lead with different degrees, and the events of lead poisoning, overproof lead content in crops and the like also occur successively. The lead pollution problem of the soil is severe day by day, and the safety of agricultural products and the health of human bodies are seriously threatened. At present, the technologies for remediating lead-polluted soil mainly comprise a soil reclamation method, a heat treatment method, an electric remediation method, a chemical fixation method, a leaching method and the like, the methods have the problems of long remediation time, high cost, secondary pollution and the like, the plant extraction remediation by using plants has the advantages of environmental friendliness, no secondary pollution and the like and is favored by academia, but the plant remediation efficiency is influenced by the low effectiveness of lead in the soil, so that the development of an inexpensive, efficient and environment-friendly activating agent is necessary.
The chelating agent can be used for activating soil heavy metals and improving the plant extraction efficiency, and is divided into a natural chelating agent and an artificial chelating agent. In recent 20 years, artificially synthesized chelating agents represented by ethylenediaminetetraacetic acid (EDTA) have been widely used to enhance plant extraction efficiency and achieve certain effects, but EDTA is not easily biodegradable and is likely to cause secondary pollution. Some easily degradable green natural chelating agents such as glutamic acid N, N-acetyl acetic acid tetrasodium (GLDA) and nitrilotriacetic acid (NTA) improve the plant extraction efficiency and are gradually hot spots in the research of plant repair. However, the lead activation efficiency of the chelating agents is low, so that the popularization and the application of the chelating agents are limited.
The low molecular weight organic acid such as citric acid, oxalic acid and the like has the function of activating heavy metals, is environment-friendly, can be biologically degraded and the like, and has an important function in the activation of the heavy metals in the soil. However, the method of using artificially synthesized organic acid to activate and extract plants has high cost and the effect of the method is influenced by the types of plants and heavy metals.
Disclosure of Invention
The invention aims to solve the technical problem of overcoming the defects in the prior art and provides a preparation method of a heavy metal activator for activating lead-polluted soil. The heavy metal activator is environment-friendly, wide in source and convenient to synthesize.
In order to solve the technical problem, the technical scheme adopted by the invention is as follows:
the preparation method of the plant source soil heavy metal activator for the lead-contaminated soil is provided, and comprises the following steps:
(1) taking fresh lemon peel, and mincing to obtain lemon peel residue;
(2) adding the ultrapure water into the lemon peel residues for several times under stirring, wherein the mass ratio of the lemon peel residues to the water is 1: 4; after being uniformly stirred, the mixture and the container are placed in a reciprocating type oscillator for oscillation treatment, then centrifugal separation is carried out, and supernatant is taken and filtered;
(3) adding a chelating agent GLDA solution and a biosurfactant tea saponin solution into the filtered supernatant, and then placing the container in a reciprocating type oscillator for oscillation treatment;
the volume ratio of the supernatant to the GLDA solution to the tea saponin solution is 15: 2.5; wherein the mass concentration of the chelating agent GLDA solution is 0.7%, and the mass concentration of the tea saponin solution is 4%;
(4) adjusting the pH value of the mixed solution after the oscillation treatment to be 4, and keeping the mixed solution in a dark place and in a sealed way.
In the invention, when the oscillation treatment is carried out in the steps (2) and (3), the oscillation frequency is 250r/min, the time is 30min, and the temperature is 20 ℃.
In the invention, when the centrifugal separation is carried out in the step (2), the rotating speed of the centrifugal machine is 5000r/min, the time is 15min, and the temperature is 20 ℃.
In the present invention, in step (4), the pH of the mixed solution is adjusted using a 0.1mol/L HCl solution or NaOH solution.
Description of the inventive principles:
the invention seeks a novel activating agent which is wide in source, environment-friendly, low in cost and mainly comprises fruit residues, can activate lead in soil, does not cause environmental pollution, and simultaneously realizes resource utilization of wastes.
The lemon is rich in citric acid, total saponin, limonin and other active substances, the activation efficiency on heavy metals is remarkable, and the lemon peel residue is used as a residual waste resource of fresh lemon juice, so that the cost is low, and the lemon is green and environment-friendly. Tea saponin is a biosurfactant and is also a main substance for repairing heavy metals. It can remove acid soluble and reducible heavy metals in soil, and has the characteristics of reducing solution surface tension, good wettability, penetrability, emulsifying dispersibility and the like, and is easy to degrade, easy to prepare, wide in source, low in price and the like when used in a large amount in the environment. Therefore, the lemon peel residues are fully utilized as the main material, the extracting solution containing active ingredients such as citric acid is obtained by optimizing the extraction process, and the extracting solution is matched with the natural chelating agent and the biosurfactant, so that the novel heavy metal activator can be prepared, and the resource utilization of wastes can be realized.
The contents of heavy metal ions and organic matters in the ultrapure water are extremely high, the interference of the heavy metal ions is eliminated, the chelation complexing effect of the organic matters on the ions in the extraction solution is reduced, and the pH value is stable at 6.8-7.
Compared with the prior art, the invention has the beneficial effects that:
1. the activating agent of the invention has wide raw material source and low price.
2. The preparation method is simple and consumes short time.
3. The activating agent is green and environment-friendly, and does not cause secondary pollution.
Drawings
FIG. 1 is a graph comparing the efficiency of heavy metal activation with different reagents.
The histograms in the figure are represented in sequence as: the mixture of single chelating agent EDTA, lemon peel residue supernatant, GLDA solution and tea saponin solution according to different volume ratios.
Detailed Description
In order to make the present invention more comprehensible, the technical solutions of the present invention are further described below with reference to specific embodiments, but the present invention is not limited thereto.
The preparation method of the heavy metal activator for activating the lead-polluted soil comprises the following steps:
(1) taking fresh lemon peel, and mincing to obtain lemon peel residue;
(2) adding the ultrapure water into the lemon peel residues for several times under stirring, wherein the mass ratio of the lemon peel residues to the water is 1: 4; after being uniformly stirred, the mixture and the container are placed in a reciprocating type oscillator for oscillation treatment, then centrifugal separation is carried out, and supernatant is taken and filtered; the oscillation frequency of the oscillation treatment is 250r/min, the time is 30min, and the temperature is 20 ℃; the rotation speed of the centrifuge is 5000r/min, the time is 15min, and the temperature is 20 ℃;
(3) adding a chelating agent GLDA solution and a biosurfactant tea saponin solution into the filtered supernatant, and then placing the container in a reciprocating type oscillator for oscillation treatment;
the volume ratio of the supernatant to the GLDA solution to the tea saponin solution is 15: 2.5; wherein the mass concentration of the chelating agent GLDA solution is 0.7%, and the mass concentration of the tea saponin solution is 4%;
(4) adjusting the pH value of the mixture after the oscillation treatment to 4 by using 0.1mol/L hydrochloric acid, and keeping the mixture in a dark place and in a sealed way.
The following are specific examples of applications for heavy metal activators:
1. performing an orthogonal experiment to determine the optimal experimental conditions for soil heavy metal activation:
when the activating agent is applied to lead activation treatment of lead-containing soil, the activating agent specifically comprises the following steps: weighing about 1.000g of soil sample into a 50ml centrifuge tube, adding 20ml of the plant source soil heavy metal activator prepared by the invention into the corresponding centrifuge tube, and placing the centrifuge tube into an oscillator for oscillation (200r/min, 12h, 25 ℃). And then centrifuging the vibrated centrifuge tube at room temperature for 15 minutes at 5000r/min, taking supernate, adding 5ml of concentrated nitric acid, digesting and digesting the organic matter, filtering the digested liquid through a 0.45-micron filter membrane, and measuring the concentration of the solution lead by utilizing ICP-OES.
Taking at least 9 groups of identical and equal lead-polluted soil, carrying out a lead activation experiment on the lead-polluted soil by using an equal amount of an activating agent for each group of soil, and carrying out orthogonal experiment design according to temperature, oscillation time and initial pH; wherein, the temperature refers to the oscillation temperature when different reagents are mixed in the experiment, the oscillation time refers to the oscillation time when different reagents are mixed in the experiment, and the initial pH refers to the pH of an initial solution after an activating agent is mixed in the experiment; the experiment adopts the oscillation temperature of 10 ℃, 20 ℃, 30 ℃, the oscillation time of 12h, 24h and 36h and the initial pH of 3, 4 and 5 to carry out orthogonal experiment design. After the experiment is finished, selecting a group with the highest soil lead activation rate, and determining the oscillation temperature, the oscillation time and the initial pH of the group as the optimal experiment conditions; the optimal experimental conditions for the final determination were a shaking temperature of 20 ℃, a shaking time of 24h and an initial pH of 4.
Example 1:
when the experiment for activating the soil lead by using the activating agent is carried out, the optimal oscillation temperature, the optimal oscillation time and the initial optimal pH value of a prepared reagent need to be determined by using an orthogonal experiment, at least 9 groups of identical and equal soil polluted by lead are taken, and the identical and equal activating agent is used for each group of soil to carry out the soil lead activation experiment. According to the experimental results in table 1, the activation rate of lead in the 5 th group of soil in 9 groups of experiments is 57.8% at the highest, and further, the optimal experimental conditions are determined to be that the oscillation temperature is 20 ℃, the oscillation time is 24h, and the initial pH is 4.
TABLE 1 results of orthogonal experiments
2. Under the determined optimal experimental conditions, at least 3 comparative concentration values are determined for EDTA, GLDA and tea saponin respectively, and the comparative experiment of the activating effect of the activating agent on the lead is carried out respectively.
a: taking at least 27 groups of identical and equivalent lead-polluted soil, and respectively adopting 0.06mol/L, 0.08mol/L and 0.1mol/L of Ethylene Diamine Tetraacetic Acid (EDTA) with solution concentration being the comparative concentration value according to the respective determined comparative concentration value; the mass concentration of the glutamic acid, N, N-acetyl acetic acid tetrasodium (GLDA) solution is 0.5%, 0.6% and 0.7%; performing a soil lead activation experiment of a single activator on the tea saponin solution with the mass concentration of 2%, 3% and 4%, and recording the soil lead activation rate of each group;
b: taking at least 15 groups of identical and equal lead-polluted soil, and respectively adopting a compound activator with solution concentration as a comparative concentration value according to the respective determined comparative concentration value to carry out a soil lead activation experiment, wherein the compound activator is as follows: fixing the lemon residue extract into a compound desorbent with the volume ratio of GLDA to tea saponin being 8:2, 6:4, 5:5, 4:6 and 2:8 of the volume of an activating agent, and recording the lead activation rate of the soil after the experiments of each group are finished;
after the experiment is finished, the concentration values are selected to be 0.08mol/L of the Ethylene Diamine Tetraacetic Acid (EDTA), 0.7 mass percent of the glutamic acid N, N-acetyl acetic acid tetrasodium (GLDA) and 4 mass percent of the tea saponin.
3. And C, comparing the lead activation rates of the soil after the experiments of the groups in the step B, and selecting the group with the highest lead activation rate of the soil, wherein the volume ratio and the concentration of the compound activating agents of the group are the preparation results of the novel compound activating agents for treating the lead-polluted soil.
After the experiment is finished, the activator is determined to be composed of the lemon peel residue extract, the GLDA and the tea saponin, the volume ratio of the lemon peel residue extract to the GLDA to the tea saponin is 15:2.5:2.5, the mass concentration of the GLDA solution is 0.7%, and the mass concentration of the tea saponin solution is 4%.
The chelating agent GLDA used in the experiments was purchased from Acksonobel and had a solids content of about 47% and a density of 1.4g/cm3And an average molecular weight of 351.1, wherein CAS number is 51981-21-6.
3. Preparation and application of heavy metal activator
And (3) putting the lemon peel residues into a stirrer, adding the added ultrapure water in four times on average at intervals of 30s every time, wherein the mass ratio of the ultrapure water to the lemon peel residues is 4:1, and uniformly stirring to obtain the lemon peel residue extract. Placing into a 50ml centrifuge tube, shaking at 20 deg.C at 250r/min for 30 min. Then placing the mixture into a high-speed centrifuge for centrifugation, centrifuging the mixture at a high speed of 5000r/min for 15min at the temperature of 20 ℃, and then taking supernate to pass through a 0.45 mu m filter membrane. Mixing the filtered supernatant with a GLDA solution and a tea saponin solution according to the volume ratio of 15: 2.5; wherein the mass concentration of the chelating agent GLDA solution is 0.7%, and the mass concentration of the tea saponin solution is 4%; then placing into a reciprocating type oscillator, and oscillating at the frequency of 250r/min for 30min at the temperature of 20 ℃. And (3) adjusting the pH of the mixed solution to 4 by using 0.1mol/L HCL solution or NaOH solution to obtain the compound activator.
Example 2:
the preparation method of the soil heavy metal activator comprises the following steps:
1) and (3) putting 50g of lemon peel residues into a stirrer, adding 200g of ultrapure water four times on average at intervals of 30s every time, and uniformly stirring to obtain the lemon peel residue extract.
2) Placing the lemon peel residue extract into a 50ml centrifuge tube, shaking at 20 deg.C at 250r/min for 30 min. Then placing the mixture into a high-speed centrifuge for centrifugation, centrifuging the mixture for 15min at the temperature of 20 ℃ at 5000r/min, and then removing supernatant and filtering the supernatant through a 0.45 mu m filter membrane.
3) Mixing the supernatant with 0.7% GLDA solution and 4% tea saponin solution at volume ratio of 15:2.5, 15: 4:1 and 15: 1: 4 respectively to obtain 20ml of mixture, and placing into a reciprocating shaker at 20 deg.C and 200r/min for 24 hr.
4) The mixed solution was taken and the initial pH of the mixed solution was adjusted to 4 with 0.1mol/L HCl.
The novel soil heavy metal activator prepared by the method is used for treating the soil polluted by high-concentration lead, and the liquid-soil ratio of the activator to the soil is 20: 1. The results showed that the activators obtained in example 2 had lead-activating rates of 57.1%, 44.6% and 39.8%, respectively, whereas as can be seen from fig. 1, the lead-activating rate of EDTA alone was 67.8% and the lead-activating rate of lemon peel residue extract alone was 33.6%. Therefore, the novel activating agent provided by the invention can ensure a certain high-efficiency activating efficiency, simultaneously avoid secondary pollution to the environment, is low in price and easy to prepare, and achieves the purpose of recycling waste.
Claims (1)
1. A preparation method of a plant source soil heavy metal activator for lead contaminated soil is characterized by comprising the following steps:
(1) taking fresh lemon peel, and mincing to obtain lemon peel residue;
(2) adding the ultrapure water into the lemon peel residues for several times under stirring, wherein the mass ratio of the lemon peel residues to the water is 1: 4; after being uniformly stirred, the mixture and the container are placed in a reciprocating type oscillator for oscillation treatment, then centrifugal separation is carried out, and supernatant is taken and filtered; the rotation speed of the centrifuge is 5000r/min, the time is 15min, and the temperature is 20 ℃;
(3) adding a chelating agent GLDA solution and a biosurfactant tea saponin solution into the filtered supernatant, and then placing the container in a reciprocating type oscillator for oscillation treatment;
the volume ratio of the supernatant to the GLDA solution to the tea saponin solution is 15: 2.5; wherein the mass concentration of the chelating agent GLDA solution is 0.7%, and the mass concentration of the tea saponin solution is 4%;
(4) adjusting the pH value of the mixed solution subjected to oscillation treatment to be 4 by using 0.1mol/L HCL solution or NaOH solution, and keeping the mixed solution in a dark place and in a sealed way;
during the oscillation treatment in the steps (2) and (3), the oscillation frequency is 250r/min, the time is 30min, and the temperature is 20 ℃.
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