CN113174265A - Composite heavy metal contaminated soil remediation agent and preparation method thereof - Google Patents
Composite heavy metal contaminated soil remediation agent and preparation method thereof Download PDFInfo
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- CN113174265A CN113174265A CN202110423198.4A CN202110423198A CN113174265A CN 113174265 A CN113174265 A CN 113174265A CN 202110423198 A CN202110423198 A CN 202110423198A CN 113174265 A CN113174265 A CN 113174265A
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- water
- heavy metal
- rubber
- contaminated soil
- soil remediation
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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
- C09K17/40—Soil-conditioning materials or soil-stabilising materials containing mixtures of inorganic and organic compounds
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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
Abstract
The invention belongs to the technical field of environment-friendly materials, and particularly relates to a composite heavy metal contaminated soil remediation agent and a preparation method thereof. The product developed by the invention comprises nano elastomer particles; the nano elastomer particles are of hollow structures; the nano elastomer particles comprise water-swelling rubber and graphene oxide; the water-swelling rubber comprises polar rubber and water-absorbing resin; the polar rubber is selected from at least one of nitrile rubber or chloroprene rubber. During preparation, the water-absorbing resin and the graphene oxide are ultrasonically dispersed in water to obtain an aqueous phase dispersion liquid; mixing and swelling polar rubber and methylbenzene, and performing ultrasonic dispersion to obtain an oil phase dispersion liquid; then shearing and dispersing the aqueous phase dispersion liquid and the oil phase dispersion liquid at a speed of more than 20000r/min at a high speed to obtain a coarse emulsion; and then homogenizing the crude emulsion under high pressure, and spray drying to obtain the hollow nano elastomer particles.
Description
Technical Field
The invention belongs to the technical field of environment-friendly materials. More particularly relates to a composite heavy metal contaminated soil remediation agent and a preparation method thereof.
Background
The heavy metal sources in the soil are mainly two: the biomass naturally flows in, namely weathered decomposition of the mature soil mother rock and rotten decomposition of the withered biomass flow into soil under natural conditions to cause heavy metal enrichment of the soil; the second is heavy metal that human activities flow in, that is, the accumulation of heavy metal in soil caused by human in the processes of mineral resource development, industrial development, agricultural production and the like, which is the most main cause of heavy metal pollution of soil. The contamination produced in the production of industrial products is as follows: the manufacturing process of products such as three wastes, metallurgy, oil refining, electronic manufacturing and the like can cause heavy metal pollution to soil; agricultural wastes such as pesticides and chemical fertilizers applied in agricultural production can also pollute the heavy metals in the soil; heavy metal dust scattered in the transportation process can also cause damage to soil.
Common heavy metal restoration agents are classified into: inorganic repairing agent and organic repairing agent, the inorganic repairing agent is lime, flyash, hydroxyapatite, calcium magnesium phosphate fertilizer and other matter and contains bentonite. The organic repairing agent component relates to biological carbon, organic fertilizer and sludge.
Lime is one of the most widely used heavy metal remediation agents at present. Research shows that the pH value of the soil and the content of the chromium in the available state of the soil are in negative correlation (p is less than 0.05), so that the content of the chromium in the available state of the soil can be reduced by applying lime to improve the pH value of the soil. The lime is applied to increase the accumulation amount of Cd in root systems, so that the ratio of Cd content in the root systems of plants to that in the overground part is remarkably increased. However, lime alone only raises the pH of the soil, but when the environment changes, the deactivated metal ions may be released.
The organic fertilizer applied to the soil can provide sufficient nutrient components for plants, such as carbon-containing materials from plants and animals. Researches show that the organic fertilizer can reduce the bioavailability of Cd and Zn in the composite polluted red soil, and by applying the organic fertilizer, the Cd and Zn in the soil are converted into a form which is not easy to be absorbed by plants, and the content of heavy metal in the effective state of the soil which has good correlation with the growth of the plants is obviously reduced. The pig manure can prevent heavy metals such as Cd, Pb, Cu and the like from transferring from the lower part to the upper part of the plant, so that the content of chlorophyll in the plant is increased, for example, the biomass can be improved by applying 10kg of the pig manure, but the pig manure is not suitable for being used in large quantity, and the total amount of the heavy metals in the soil can be increased to a certain extent because the organic fertilizer contains a small amount of heavy metals, so that the effective state of the heavy metals in the soil is also influenced to a certain extent.
Disclosure of Invention
The invention aims to overcome the defect that the adsorption and repair capacity of a product to heavy metal ions in soil is insufficient due to the fact that the existing single heavy metal soil repair agent is limited by soil resistance and uneven distribution of the heavy metal ions in the soil in the using process, and provides a composite heavy metal polluted soil repair agent and a preparation method thereof.
The invention aims to provide a composite heavy metal contaminated soil remediation agent.
The invention also aims to provide a preparation method of the composite heavy metal contaminated soil remediation agent.
The above purpose of the invention is realized by the following technical scheme:
a composite heavy metal contaminated soil remediation agent, comprising: nano-elastomer particles;
the nano elastomer particles are of hollow structures;
the nano elastomer particles comprise water-swelling rubber and graphene oxide;
the water-swelling rubber comprises polar rubber and water-absorbing resin;
the polar rubber is selected from at least one of nitrile rubber or chloroprene rubber.
According to the technical scheme, nano-grade elastomer particles are selected as effective components of the soil remediation agent, and a hollow structure constructed by water-absorbing swelling rubber and graphene oxide is used as the nano-elastomer particles, wherein the water-absorbing swelling rubber comprises polar rubber and water-absorbing resin; in the use process of an actual product, along with the scouring action of rainwater and the like, the nano elastomer particles firstly utilize the smaller size of the nano elastomer particles to quickly diffuse and permeate in soil, along with the time prolongation, the water-absorbent resin can absorb the water in the soil, and the water enters the rubber molecules through physical actions such as diffusion, capillarity, surface adsorption and the like to form stronger affinity with hydrophilic groups in a polar rubber molecular structure, along with the continuous absorption of the water in the soil by the water-absorbent resin, the diastolic expansion of the rubber molecular chain is caused, after the expansion, the volume of the nano elastomer particles is increased, when the water in the soil is abundant, the nano elastomer particles can float up to the surface layer of the soil, in the floating process, heavy metal ions adsorbed to each part of the soil can be intercepted, and are adsorbed and fixed in an oxidation graphene layer, and after the nano elastomer particles float up to the surface layer of the soil, with the gradual drying of moisture, the volume of the nano elastomer particles shrinks, and the heavy metal ions are fixed inside the structure of the nano elastomer particles, so that the heavy metal ions are prevented from being lost and absorbed by plants.
Furthermore, the water-swelling rubber also comprises tackifying resin accounting for 5-10% of the mass of the polar rubber.
According to the technical scheme, tackifying resin is further introduced, so that the physical structure stability of the nano elastomer particles in the water-absorbing expansion process can be improved, and desorption of adsorbed heavy metal ions caused by weak structure collapse in the full water-absorbing expansion and contraction processes is avoided.
Further, the tackifying resin is selected from at least one of C5 petroleum resin, C9 petroleum resin and terpene resin.
Further, an anionic surfactant is dispersed in the hollow structure of the nano elastomer particle.
By introducing the anionic surfactant into the hollow structure in the nano elastomer particles, firstly, the anionic surfactant is positioned in the particles, so that the electrostatic effect can be generated on heavy metal ions adsorbed on the surface layer or between graphene oxide layers, and the adsorption and fixation capacity on the heavy metal ions can be further enhanced; and secondly, the existence of the surfactant is beneficial to ensuring that a hollow structure is formed in the preparation process, so that the nano elastomer particles can be flexibly diffused and permeated in the soil by utilizing the water absorption expansion of the water absorption expansion rubber.
Further, the anionic surfactant is selected from at least one of anionic polyacrylamide, higher fatty acid sodium, sodium dodecyl benzene sulfonate, sodium lignin sulfonate and sodium lauryl sulfate.
Further, the water-absorbing resin is selected from at least one of sodium polyacrylate, isobutylene-maleic anhydride copolymer and polyvinyl alcohol/acrylate graft copolymer.
A preparation method of a composite heavy metal contaminated soil remediation agent comprises the following specific preparation steps:
(1) ultrasonically dispersing water-absorbent resin and graphene oxide in water to obtain an aqueous phase dispersion liquid;
(2) mixing and swelling polar rubber and methylbenzene, and performing ultrasonic dispersion to obtain an oil phase dispersion liquid;
(3) shearing and dispersing the aqueous phase dispersion liquid and the oil phase dispersion liquid at a speed of more than 20000r/min at a high speed to obtain a coarse emulsion;
(4) and (3) homogenizing the coarse emulsion under high pressure, and then carrying out spray drying to obtain the hollow nano elastomer particles.
Further, the specific preparation steps further comprise:
in the step (2), tackifying resin with the mass of 5-10% of that of the polar rubber is added.
Further, the specific preparation steps further comprise:
in the step (1), an anionic surfactant is added.
Detailed Description
The present invention is further illustrated by the following specific examples, which are not intended to limit the invention in any way. Reagents, methods and apparatus used in the present invention are conventional in the art unless otherwise indicated.
Unless otherwise indicated, reagents and materials used in the following examples are commercially available.
Example 1
According to the weight parts, sequentially taking 10 parts of water-absorbent resin, 10 parts of graphene oxide, 40 parts of polar rubber, 4 parts of anionic surfactant, 200 parts of water, 150 parts of toluene and tackifying resin accounting for 5% of the mass of the polar rubber;
firstly, mixing water-absorbing resin, graphene oxide, an anionic surfactant and water, standing and swelling for 8 hours at room temperature, and after swelling is finished, carrying out constant-temperature ultrasonic dispersion for 4 hours at the temperature of 55 ℃ and the ultrasonic frequency of 80kHz to obtain an aqueous phase dispersion liquid;
standing and swelling polar rubber, tackifying resin and toluene at the temperature of 45 ℃ for 24 hours, and then ultrasonically dispersing at the constant temperature of 75 ℃ and the ultrasonic frequency of 150kHz for 4 hours to obtain an oil phase dispersion liquid;
mixing an aqueous phase dispersion liquid and an oil phase dispersion liquid according to a mass ratio of 1: 1, mixing and pouring the mixture into a high-speed dispersion machine, and carrying out constant-temperature high-speed shearing dispersion for 2 hours at the temperature of 75 ℃ and the rotating speed of 20000r/min to obtain a coarse emulsion;
transferring the crude emulsion into a high-pressure homogenizing pot, homogenizing for 4 times under 100MPa for 20min, and discharging to obtain nanometer emulsion;
conveying the nano emulsion into a spray dryer, spray drying and discharging under the conditions that the air inlet temperature is 120 ℃, the air outlet temperature is 75 ℃ and the feeding rate is 30g/min to obtain hollow nano elastomer particles which can be used as a component of a composite heavy metal contaminated soil remediation agent;
the tackifying resin is C5 petroleum resin;
the anionic surfactant is anionic polyacrylamide;
the water-absorbing resin is sodium polyacrylate;
the polar rubber is nitrile rubber.
Example 2
According to the weight parts, 15 parts of water-absorbent resin, 12 parts of graphene oxide, 45 parts of polar rubber, 5 parts of anionic surfactant, 250 parts of water, 180 parts of toluene and tackifying resin accounting for 7% of the mass of the polar rubber are taken in sequence;
firstly, mixing water-absorbing resin, graphene oxide, an anionic surfactant and water, standing and swelling for 10 hours at room temperature, and after swelling is finished, carrying out constant-temperature ultrasonic dispersion for 5 hours at the temperature of 65 ℃ and the ultrasonic frequency of 100kHz to obtain an aqueous phase dispersion liquid;
standing and swelling polar rubber, tackifying resin and toluene at the temperature of 48 ℃ for 32 hours, and then ultrasonically dispersing at the constant temperature of 78 ℃ and the ultrasonic frequency of 180kHz for 5 hours to obtain an oil phase dispersion liquid;
mixing an aqueous phase dispersion liquid and an oil phase dispersion liquid according to a mass ratio of 1.1: 1, mixing and pouring the mixture into a high-speed dispersion machine, and carrying out constant-temperature high-speed shearing dispersion for 3 hours at the temperature of 80 ℃ and the rotating speed of 25000r/min to obtain a coarse emulsion;
transferring the crude emulsion into a high-pressure homogenizing pot, homogenizing at 110MPa for 5 times with single time of 25min, and discharging to obtain nanometer emulsion after high-pressure homogenization;
conveying the nano emulsion into a spray dryer, spray drying and discharging under the conditions that the air inlet temperature is 125 ℃, the air outlet temperature is 80 ℃ and the feeding rate is 40g/min to obtain hollow nano elastomer particles which can be used as a component of a composite heavy metal contaminated soil remediation agent;
the tackifying resin is C9 petroleum resin;
the anionic surfactant is sodium dodecyl benzene sulfonate;
the water-absorbing resin is an isobutylene-maleic anhydride copolymer;
the polar rubber is nitrile rubber.
Example 3
According to the weight parts, sequentially taking 20 parts of water-absorbent resin, 15 parts of graphene oxide, 50 parts of polar rubber, 6 parts of anionic surfactant, 300 parts of water, 200 parts of toluene and tackifying resin accounting for 10% of the mass of the polar rubber;
firstly, mixing water-absorbing resin, graphene oxide, an anionic surfactant and water, standing and swelling for 12 hours at room temperature, and after swelling is finished, carrying out constant-temperature ultrasonic dispersion for 6 hours at the temperature of 75 ℃ and the ultrasonic frequency of 120kHz to obtain an aqueous phase dispersion liquid;
standing and swelling polar rubber, tackifying resin and toluene at 50 ℃ for 36h, and performing constant-temperature ultrasonic dispersion at 80 ℃ and ultrasonic frequency of 200kHz for 6h to obtain an oil phase dispersion liquid;
mixing the aqueous phase dispersion liquid and the oil phase dispersion liquid according to the mass ratio of 1.2: 1, mixing and pouring the mixture into a high-speed dispersion machine, and carrying out constant-temperature high-speed shearing dispersion for 4 hours at the temperature of 85 ℃ and the rotating speed of 30000r/min to obtain a coarse emulsion;
transferring the crude emulsion into a high-pressure homogenizing pot, homogenizing for 6 times under 120MPa for 30min, and discharging to obtain nanometer emulsion;
conveying the nano emulsion into a spray dryer, spray drying and discharging under the conditions that the air inlet temperature is 130 ℃, the air outlet temperature is 85 ℃ and the feeding speed is 50g/min to obtain hollow nano elastomer particles which can be used as a component of a composite heavy metal polluted soil repairing agent;
the tackifying resin is terpene resin;
the anionic surfactant is sodium lignosulfonate;
the water-absorbing resin is a polyvinyl alcohol/acrylate graft copolymer;
the polar rubber is chloroprene rubber.
Example 4
This example differs from example 1 in that: no tackifying resin was added and the remaining conditions were kept unchanged.
Example 5
This example differs from example 1 in that: the remaining conditions were kept constant for the addition of anionic surfactant.
Comparative example 1
This comparative example differs from example 1 in that: no water-absorbing resin was added, and the remaining conditions were maintained.
Comparative example 2
This comparative example differs from example 1 in that: no polar rubber was added and the remaining conditions were kept constant.
The products obtained in examples 1-5 and comparative examples 1-2 were tested for their performance, and the specific test methods and test results are as follows:
the experiment is carried out by adopting pollution-free soil and adding chromium nitrate to prepare heavy metal polluted soil. After dissolving the chromium nitrate in water, uniformly irrigating the soil without pollution. In order to shorten the experimental time, the soil added with the pollutants is placed in a constant-temperature constant-humidity incubator for aging treatment, and the aging time is 40 days. Measuring the initial concentration of chromium ions in the self-made polluted soil to be 1052.5 mg/kg;
according to the addition amount of 10% of the soil mass, adding the products of the above embodiments and comparative examples into the soil with equal mass and added with pollutants respectively, spraying water to the surface layer of the soil, wherein the water spraying amount is 40% of the soil mass, after the water spraying is finished, irradiating for 3 hours under the condition that the sunlight intensity is 3 kalx, spraying water in such a circulating manner, after irradiating for 5 times, testing the concentration of chromium ions in the soil, and calculating the removal rate of the chromium ions;
| chromium ion removal rate/%) | |
| Example 1 | 75.6 |
| Example 2 | 74.2 |
| Example 3 | 77.6 |
| Example 4 | 66.1 |
| Example 5 | 67.5 |
| Comparative example 1 | 23.6 |
| Comparative example 2 | 32.2 |
The test results in table 1 show that the product obtained by the invention can effectively utilize the change of water in soil and has excellent adsorption performance on heavy metal ions in soil.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (9)
1. The compound heavy metal contaminated soil remediation agent is characterized by comprising the following components in parts by weight: nano-elastomer particles;
the nano elastomer particles are of hollow structures;
the nano elastomer particles comprise water-swelling rubber and graphene oxide;
the water-swelling rubber comprises polar rubber and water-absorbing resin;
the polar rubber is selected from at least one of nitrile rubber or chloroprene rubber.
2. The compound heavy metal contaminated soil remediation agent of claim 1, wherein: the water-swelling rubber also comprises tackifying resin accounting for 5-10% of the mass of the polar rubber.
3. The compound heavy metal contaminated soil remediation agent of claim 2, wherein: the tackifying resin is at least one selected from C5 petroleum resin, C9 petroleum resin and terpene resin.
4. The compound heavy metal contaminated soil remediation agent of claim 1, wherein: the hollow structure of the nano elastomer particles is dispersed with an anionic surfactant.
5. The compound heavy metal contaminated soil remediation agent of claim 4, wherein: the anionic surfactant is selected from at least one of anionic polyacrylamide, higher fatty acid sodium, sodium dodecyl benzene sulfonate, sodium lignin sulfonate and sodium lauryl sulfate.
6. The compound heavy metal contaminated soil remediation agent of claim 1, wherein: the water-absorbing resin is at least one selected from sodium polyacrylate, isobutylene-maleic anhydride copolymer and polyvinyl alcohol/acrylate graft copolymer.
7. A preparation method of a composite heavy metal contaminated soil remediation agent is characterized by comprising the following specific preparation steps:
(1) ultrasonically dispersing water-absorbent resin and graphene oxide in water to obtain an aqueous phase dispersion liquid;
(2) mixing and swelling polar rubber and methylbenzene, and performing ultrasonic dispersion to obtain an oil phase dispersion liquid;
(3) shearing and dispersing the aqueous phase dispersion liquid and the oil phase dispersion liquid at a speed of more than 20000r/min at a high speed to obtain a coarse emulsion;
(4) and (3) homogenizing the coarse emulsion under high pressure, and then carrying out spray drying to obtain the hollow nano elastomer particles.
8. The method for preparing a composite heavy metal contaminated soil remediation agent of claim 7, wherein the steps of preparing further comprise:
in the step (2), tackifying resin with the mass of 5-10% of that of the polar rubber is added.
9. The method for preparing a composite heavy metal contaminated soil remediation agent of claim 7, wherein the steps of preparing further comprise:
in the step (1), an anionic surfactant is added.
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Application publication date: 20210727 |