CN111821910A - Amphiphilic surfactant, eluting agent and application thereof - Google Patents
Amphiphilic surfactant, eluting agent and application thereof Download PDFInfo
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- CN111821910A CN111821910A CN201910319443.XA CN201910319443A CN111821910A CN 111821910 A CN111821910 A CN 111821910A CN 201910319443 A CN201910319443 A CN 201910319443A CN 111821910 A CN111821910 A CN 111821910A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
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- B09C1/00—Reclamation of contaminated soil
- B09C1/08—Reclamation of contaminated soil chemically
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Abstract
The invention discloses an amphiphilic surfactant, an eluting agent and application thereof. The amphiphilic surfactant is a nano graphene oxide dispersion liquid grafted with a long alkyl chain; the structure is that one side of the nano graphene oxide is grafted with a long alkyl chain. The surfactant provided by the invention has amphiphilicity, can enter the middle of soil and petroleum hydrocarbon, and reduces the adsorbability of the petroleum hydrocarbon and the soil, thereby playing a role in solubilization. The main component of the amphiphilic surfactant is composed of hydrocarbon elements, and the amphiphilic surfactant is environment-friendly, easy to degrade and free of secondary environmental pollution.
Description
Technical Field
The invention relates to the field of soil remediation, in particular to an amphiphilic surfactant, an eluting agent and application thereof.
Background
With the rapid development of the oil industry, the pollution of oil field exploitation to soil is more and more serious. After entering the soil, petroleum pollutants not only destroy the structure of the soil and change the physical and chemical properties of the soil, but also affect the yield and quality of crops and endanger the health and life of human beings through the food chain. Therefore, repairing contaminated soil and ensuring human health have attracted extensive attention of governments and environmentalists of various countries and become a hot spot of current domestic and foreign environmental research.
The soil pollution remediation technology is a general term for technologies that adopt chemical, physical and biological technologies and methods to reduce the concentration of pollutants in soil, fix soil pollutants, convert the soil pollutants into low-toxicity or non-toxic substances and block the transfer pathway of the soil pollutants in an ecosystem. Among them, chemical leaching is one of the relatively mature technologies for treating petroleum hydrocarbon pollution at present.
Chemical leaching, namely, pushing a leaching solution to be injected into a polluted soil layer under the action of gravity or through water head pressure by means of a chemical/biochemical solvent capable of promoting the dissolution or migration of pollutants in the soil environment, and then extracting the solution containing the pollutants from the soil for separation and sewage treatment. Can remove hydrocarbon compounds such as heavy metals, aromatic hydrocarbons, petroleum and the like and halides such as TCE, polychlorinated biphenyl, chlorophenol and the like in soil, and the main leacheate comprises: clear water, inorganic solvent, chelating agent, surfactant and the like, wherein the surfactant is most widely applied.
The prior surfactant has the following defects:
the soil has large adsorption capacity to the surface active agent, and the surface active agent is not easy to desorb after being adsorbed, and the artificially synthesized surface active agent contains environmental hormone substances, has biotoxicity, is easy to cause secondary pollution, and simultaneously needs higher treatment temperature, thus increasing the difficulty of operation.
Therefore, the novel eluting agent which has good biocompatibility and easy degradation and can efficiently remove the petroleum hydrocarbon in the soil is developed, and the novel eluting agent has important significance for the subsequent reclamation or reutilization of the soil.
Disclosure of Invention
Objects of the invention
The invention aims to provide an amphiphilic surfactant, an eluting agent and application thereof, wherein the surfactant has amphiphilicity, can enter the middle of soil and petroleum hydrocarbon, reduces the adsorbability of the petroleum hydrocarbon and the soil, and can play a role in solubilization.
(II) technical scheme
In order to solve the above problems, a first aspect of the present invention provides an amphiphilic surfactant, which is nano graphene oxide grafted with a long alkyl chain; the structure is that one side of the nano graphene oxide is grafted with a long alkyl chain.
Further, the long alkyl chain is: one or more of n-dodecyl chain, n-tetradecyl chain, n-hexadecyl chain and n-octadecyl chain.
Further, the specific surface area of the surfactant is 150-500 m2(ii)/g; and/or the particle size of the surfactant is 20nm-1000 nm.
The second aspect of the invention also provides the use of the above-mentioned amphiphilic surfactant for remediation of petroleum hydrocarbon contaminated soil.
In a third aspect of the present invention, there is also provided an eluting agent, including: the surfactant, sodium salt, potassium salt and water provided by the first aspect.
Further, the concentration of the surfactant is 0.01g/L to 0.5 g/L.
Further, the sodium salt is one or more of sodium humate, sodium bicarbonate, sodium chloride and lignin sodium; the concentration of the sodium salt is 0.05g/L-1 g/L.
Further, the potassium salt is one or more of potassium carbonate, potassium chloride, potassium sulfate and potassium borate; the concentration of the potassium salt is 0.05g/L-1 g/L.
In a fourth aspect of the invention, the application of the eluting agent provided by the third aspect is also provided, and the eluting agent is used for repairing soil polluted by petroleum hydrocarbon.
Further, the remediation step of the petroleum hydrocarbon contaminated soil comprises: spraying the eluting agent into the soil polluted by petroleum hydrocarbon, and stirring for 5-20 min; standing for 1-5 h; injecting water and stirring for 5-60 min; separating the soil from the liquid, and dehydrating the separated soil.
Further, the mass ratio of the eluting agent to the polluted soil is 5:1 kg.
Further, the soil and the liquid are separated by centrifugation, the rotation speed of the centrifugation is 500rpm-5000rpm, and the time is as follows: 3min-30 min.
(III) advantageous effects
The technical scheme of the invention has the following beneficial technical effects:
(1) the surfactant provided by the invention has amphiphilicity, can enter the middle of soil and petroleum hydrocarbon, and reduces the adsorbability of the petroleum hydrocarbon and the soil, thereby playing a role in solubilization.
(2) The amphiphilic surfactant is subjected to single-side grafting modification on the basis of graphene oxide, and the grafted side has excellent biocompatibility, is easy to carry out chemical modification and has good dispersion stability in water and physiological solution.
(3) The main component of the amphiphilic surfactant is composed of carbon, hydrogen and oxygen elements, and the amphiphilic surfactant is environment-friendly, easy to degrade and free of secondary environmental pollution.
Drawings
FIG. 1 is a schematic structural view of an amphiphilic surfactant according to a first embodiment of the present invention;
FIG. 2 is a schematic structural diagram of nano graphene oxide grafted with n-dodecyl chains according to a first embodiment of the present invention;
fig. 3 is a schematic view of a nano graphene oxide structure grafted with an n-tetradecyl chain according to a first embodiment of the present invention;
FIG. 4 is a schematic structural diagram of nano graphene oxide grafted with n-hexadecyl chains according to a first embodiment of the present invention;
fig. 5 is a schematic view of a nano graphene oxide structure grafted with n-octadecyl chains according to a first embodiment of the present invention;
FIG. 6 is a schematic flow chart of a process for preparing an amphiphilic surfactant according to a second embodiment of the present invention;
fig. 7 is a schematic flow chart of a soil remediation method according to a third embodiment of the invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be described in further detail with reference to the accompanying drawings in conjunction with the following detailed description. It should be understood that the description is intended to be exemplary only, and is not intended to limit the scope of the present invention. Moreover, in the following description, descriptions of well-known structures and techniques are omitted so as to not unnecessarily obscure the concepts of the present invention.
Before the technical scheme of the invention is explained in detail, the performance of the graphene oxide is explained. The graphene oxide has high specific surface area, excellent biocompatibility, easy chemical modification and good dispersion stability in water and physiological solution, so the graphene oxide has wide development prospect in the fields of biological nanotechnology, biomedicine and the like.
Fig. 1 is a schematic structural view of an amphiphilic surfactant according to a first embodiment of the present invention.
As shown in fig. 1, the surfactant is nano graphene oxide grafted with a long alkyl chain; the structure is that one side of the nano graphene oxide is grafted with a long alkyl chain.
The particle size of the surfactant is 20nm-1000nm, and the amphiphilicity of the surfactant is optimal in the range.
The surface grafted with the long alkyl chain of the nano graphene oxide is lipophilic, so that the surface can be better adsorbed with petroleum hydrocarbon, and the adsorption of the petroleum hydrocarbon and soil is reduced. The other surface is graphene oxide, and the hydrophilicity of the graphene oxide is reserved on the other surface, so that the surfactant has the amphiphilicity at the same time.
According to the invention, the single-side modification is carried out on the nano graphene oxide by a modification process to obtain the modified nano graphene oxide with one hydrophilic side and one oleophilic side (amphiphilic), and the modified nano graphene oxide not only inherits the characteristics of the graphene oxide, but also increases an oleophilic characteristic, so that the application field of the graphene oxide is wider. In addition, the main component of the amphiphilic surfactant is composed of hydrocarbon elements, so that the amphiphilic surfactant is environment-friendly and easy to degrade, and cannot cause secondary environmental pollution.
Optionally, the long alkyl chain is: one or more of n-dodecyl chain, n-tetradecyl chain, n-hexadecyl chain and n-octadecyl chain.
It should be noted that the longer the grafted alkyl chain, the better the lipophilic effect, but if the grafted alkyl chain is too long, the hydrophilic effect of the ungrafted surface is reduced, and therefore, the long alkyl chain is preferably a n-hexadecyl chain or a n-octadecyl chain.
Hereinafter, the amphiphilic surfactant provided in the first embodiment of the present invention will be described with reference to various examples.
Example 1
Fig. 2 is a schematic structural diagram of graphene oxide grafted with n-dodecyl chains.
As shown in FIG. 2, the surfactant is represented by graphene oxide in the middle, the lower surface is an oxygen-containing functional group in the graphene oxide, and the upper surface is grafted with n-dodecyl alkyl (-C)12H25). The specific surface area of the surfactant was 162.8m2It was found to have good adsorptivity per gram.
Example 2
Fig. 3 is a schematic structural diagram of nano graphene oxide grafted with n-tetradecyl chain.
As shown in FIG. 3, the surfactant is represented by graphene oxide in the middle, oxygen-containing functional groups in the graphene oxide on the lower surface, and n-tetradecyl chain (-C) grafted on the upper surface14H29). The specific surface area of the surfactant was 163.1m2It was found to have good adsorptivity per gram.
Example 3
Fig. 4 is a schematic structural diagram of nano graphene oxide grafted with n-hexadecyl chains.
As shown in FIG. 4, the surfactant is represented by graphene oxide in the middle, oxygen-containing functional groups in the graphene oxide on the lower surface, and n-hexadecyl chain (-C) grafted on the upper surface16H33). The specific surface area of the surfactant was 163.7m2It was found to have good adsorptivity per gram.
Example 4
Fig. 5 is a schematic structural diagram of nano graphene oxide grafted with n-octadecyl chains.
As shown in FIG. 5, the surfactant is represented by graphene oxide in the middle, oxygen-containing functional groups in the graphene oxide on the lower surface, and n-octadecyl chain (-C) grafted on the upper surface18H37). The specific surface area of the surfactant was 165.8m2It was found to have good adsorptivity per gram.
The invention also provides application of the amphiphilic surfactant to remediation of soil polluted by petroleum hydrocarbon.
Fig. 6 is a schematic flow chart of a method for preparing an amphiphilic surfactant according to a second embodiment of the present invention.
As shown in fig. 6, the method comprises the steps of:
step S101, melting 10-200 g of paraffin at 50-100 ℃, and mixing the melted paraffin with 50-500 mg of graphene oxide with the particle size of 50-500 nm, 50-500 g of water and 1-20 g of sodium chloride. The mixture was vigorously stirred at 75 ℃ to obtain a mixed solution.
Optionally, mechanical stirring can be adopted, the rotating speed is 500-2000 rpm, and the stirring time is 30-120 min.
And step S102, cooling the mixed solution to room temperature, and then carrying out centrifugal cleaning on the mixed solution by using a sodium hydroxide aqueous solution with the pH value of 8.0-14.0, water and ethanol in sequence. Obtaining a paraffin/graphene oxide mixture.
Optionally, in the centrifugal cleaning process, the rotation speed of the centrifugal machine is 500-5000 rpm, and the cleaning time is 5-50 min each time.
Step S103, adding 0.1-1.0 g of one of n-octadecyl amine, n-hexadecyl amine, n-tetradecyl amine or n-dodecyl amine into 20-500 mL of absolute ethanol, and stirring for dissolving to obtain an ethanol solution of alkylamine.
And step S104, adding the paraffin/graphene oxide mixture into an ethanol solution of alkylamine, and stirring at 20-80 ℃ to obtain an intermediate product.
Optionally, mechanical stirring can be adopted, the rotating speed is 200-1800 rpm, and the time is 3-24 hours.
And S105, adding the intermediate product into 100-1000 mL of toluene, and stirring and mixing. Mechanical stirring at a rotation speed of 50-1000 rpm can be adopted, and the stirring time is 10-200 min.
And S106, centrifugally filtering the stirred product to obtain bottom sediment, namely the amphiphilic nano graphene oxide grafted with the long alkyl chain. In the centrifugal process, the rotating speed of the centrifugal machine is 500-5000 rpm, and the time of the centrifugal machine is 5-50 min.
The amphiphilic surfactant prepared by the method is more convenient and has better effect.
Example 5
The present invention also provides an eluting agent comprising: grafted long alkyl chain nano graphene oxide, sodium salt, potassium salt and water. The eluent contains the nano graphene oxide grafted with the long alkyl chain provided by the first embodiment, and can be used for repairing petroleum hydrocarbon polluted soil.
Specifically, the concentration of the nano graphene oxide grafted with the long alkyl chain is 0.01g/L-0.5 g/L. The preferred concentration is 0.1g/L to 0.5 g/L.
It should be noted that if the concentration of the nano graphene oxide grafted with the long alkyl chain is lower than 0.01g/L, when the eluent is used, the effect of repairing the soil polluted by petroleum hydrocarbon is not obvious when the concentration is too low. If the concentration of the nano graphene oxide grafted with the long alkyl chain is higher than 0.5g/L, the nano graphene oxide particles grafted with the long alkyl chain are likely to agglomerate, and the effect of the eluent is seriously reduced.
Optionally, the sodium salt is one or more of sodium humate, sodium bicarbonate, sodium chloride and lignin sodium; the concentration of the sodium salt is 0.05g/L-1g/L, and the preferable concentration is 0.1g/L-0.5 g/L.
Optionally, the potassium salt is one or more of potassium carbonate, potassium chloride, potassium sulfate and potassium borate; the concentration of the potassium salt is 0.05g/L-1g/L, and the preferable concentration is 0.1g/L-0.5 g/L.
Fig. 7 is a schematic flow chart of a remediation method for soil contaminated with petroleum hydrocarbons according to a third embodiment of the invention.
As shown in fig. 7, the steps include step S201 to step S204:
step S201, spraying the leaching agent dispersion liquid into the soil polluted by the petroleum hydrocarbon, and stirring for 5-20 min.
Specifically, the agitation can be carried out for 5-20 minutes simultaneously with or after the spraying agent is sprayed on the soil polluted by the petroleum hydrocarbon during the spraying process of the eluting agent on the soil polluted by the petroleum hydrocarbon, so that the eluting agent and the soil polluted by the petroleum hydrocarbon are fully mixed.
And S202, standing for 1-5 h. The time for standing is preferably 2 to 3 hours.
Particularly, standing is beneficial to the nano graphene oxide grafted with long alkyl chains to enter the stone more fully
The separation effect of the petroleum hydrocarbon can be increased between the petroleum hydrocarbon and the soil.
And step S203, injecting water and stirring for 5-60 min.
Specifically, the mixture of the petroleum hydrocarbon-contaminated soil after standing and the spray-washing agent is injected into water, and stirring may be performed during or after the water injection. The standing before adding water is to allow the nano graphene oxide grafted with the long alkyl chain to enter between the petroleum hydrocarbon and the soil, and the adding water and stirring are to allow the petroleum hydrocarbon to be better separated from the soil and also have a certain solubilization effect.
In the stirring process, the nano amphiphilic graphene oxide grafted with the long alkyl chain in the eluent reduces the adsorbability of the petroleum hydrocarbon and the soil, so that the soil is separated from the petroleum hydrocarbon.
In a preferred embodiment, the weight ratio of the leaching agent dispersion to the contaminated soil is 5:1, if the mass ratio of the eluting agent to the polluted soil is higher than 5:1, the nano-amphiphilic graphite oxide particles grafted with the long chain easily agglomerate, so that the eluting effect is seriously reduced; if the mass ratio is less than 5:1, the concentration leaching effect is not obvious. Further preferably, the weight ratio of the eluting agent to the petroleum hydrocarbon polluted soil is 0.5-2: 1.
optionally, the mass ratio of the injected water to the soil polluted by the petroleum hydrocarbon is 2-3: 1.
And step S204, separating the soil from the liquid, and dehydrating the separated soil.
Specifically, the water-flooded soil is separated from the liquid, which is primarily a petroleum hydrocarbon and leachant dispersion during the process.
In one example, the soil and liquid are separated by centrifugation at 500rpm to 5000rpm for a time: 3min-30 min.
The method for repairing the soil polluted by the petroleum hydrocarbon provided by the embodiment of the invention adopts a physical method to remove the petroleum hydrocarbon in the soil, and is simple and environment-friendly.
The method provided by the above third embodiment of the present invention will be discussed in detail below in different examples.
Example 6
50mL of nano graphene oxide dispersion liquid grafted with n-hexadecyl chains and having a concentration of 0.05g/L is measured, and 20mg of sodium chloride and 50mg of potassium sulfate are respectively measured and dissolved in 50mL of water. The two were mixed to give 100mL of eluent.
100g of petroleum hydrocarbon contaminated soil was weighed and 100mL of the above eluent was added. Stirring at room temperature for 20min, and standing for 2 h.
An additional 200mL of water was added and stirred for 10 min.
And (4) carrying out centrifugal separation on the mixture stirred in the previous step at the rotating speed of 1000rpm for 10min to obtain the repaired soil at the bottom of the centrifugal tube.
And finally, dehydrating the repaired soil, and calculating to obtain the petroleum hydrocarbon removal rate of 91%.
Example 7
50mL of nano graphene oxide dispersion liquid grafted with n-dodecyl chain with the concentration of 0.1g/L is measured, and 20mg of sodium chloride and 80mg of potassium chloride are respectively weighed and dissolved in 50mL of water. The two were mixed to give 100mL of eluent.
100g of petroleum hydrocarbon contaminated soil was weighed and 100mL of the above eluent was added. Stirring at room temperature for 20min, and standing for 2 h.
200mL of water was added thereto, and the mixture was stirred for 10 min. And (4) carrying out centrifugal separation on the mixture stirred in the previous step at the rotating speed of 1000rpm for 10min to obtain the soil repaired at the bottom of the centrifugal tube.
And (4) dehydrating the repaired soil, and calculating to obtain the petroleum hydrocarbon removal rate of 80%.
Example 8
80mL of nano graphene oxide dispersion liquid grafted with the n-tetradecyl chain, the concentration of which is 0.08g/L, is weighed, and 40mg of sodium chloride and 40mg of potassium sulfate are respectively weighed and dissolved in 100mL of water. The two were mixed to give 180mL of the aqueous dispersion of the elution solvent.
200g of petroleum hydrocarbon contaminated soil was weighed and 180mL of the above eluent was added. Stirring at room temperature for 10min, and standing for 3 hr.
Then, 500mL of water was added thereto, and the mixture was stirred for 20 min. And (4) carrying out centrifugal separation on the mixture stirred in the previous step at the rotating speed of 2000rpm for 20min to obtain the soil repaired at the bottom of the centrifugal tube.
And (3) dehydrating the repaired soil, and calculating to obtain the petroleum hydrocarbon removal rate of 86%.
Example 9
80mL of nano graphene oxide dispersion liquid grafted with n-octadecyl chains and having a concentration of 0.05g/L is weighed, and 20mg of sodium bicarbonate and 40mg of potassium chloride are respectively weighed and dissolved in 40mL of water. The two were mixed to give 120mL of the aqueous dispersion of the elution solvent.
100g of petroleum hydrocarbon contaminated soil was weighed and 120mL of the above eluent was added. Stirring at room temperature for 10min, and standing for 2 h.
Then, 300mL of water was added thereto, and the mixture was stirred for 30 min. And (4) centrifugally separating the mixture stirred in the previous step at the rotating speed of 2000rpm for 30min to obtain the repaired soil at the bottom of the centrifugal tube.
And (3) dehydrating the repaired soil, wherein the petroleum hydrocarbon removal rate reaches 93 percent by calculation.
As can be seen from the above examples 6-9, the eluent provided by the present invention can enter the middle of soil and petroleum hydrocarbon, and reduce the adsorbability of the petroleum hydrocarbon and the soil, thereby achieving the effect of solubilization and having a good effect of repairing the soil polluted by the petroleum hydrocarbon.
It is to be understood that the above-described embodiments of the present invention are merely illustrative of or explaining the principles of the invention and are not to be construed as limiting the invention. Therefore, any modification, equivalent replacement, improvement and the like made without departing from the spirit and scope of the present invention should be included in the protection scope of the present invention. Further, it is intended that the appended claims cover all such variations and modifications as fall within the scope and boundaries of the appended claims or the equivalents of such scope and boundaries.
Claims (12)
1. An amphiphilic surfactant is characterized in that the surfactant is nano graphene oxide grafted with a long alkyl chain; the structure is that one side of the nano graphene oxide is grafted with a long alkyl chain.
2. The surfactant of claim 1, wherein said long alkyl chain is selected from the group consisting of: one or more of n-dodecyl chain, n-tetradecyl chain, n-hexadecyl chain and n-octadecyl chain.
3. The surfactant according to claim 1 or 2, wherein the surfactant has a specific surface area of 150 to 500m2(ii)/g; and/or
The particle size of the surfactant is 20nm-1000 nm.
4. Use of the amphiphilic surfactant of any one of claims 1-3 for remediation of petroleum hydrocarbon contaminated soil.
5. An eluting agent, which is characterized by comprising the following components: a surfactant as claimed in any one of claims 1 to 3, sodium salt, potassium salt and water.
6. The eluent according to claim 5, wherein the surfactant has a concentration of 0.01-0.5 g/L by mass/volume.
7. The eluent according to claim 5, wherein the sodium salt is selected from one or more of sodium humate, sodium bicarbonate, sodium chloride, sodium lignose; the mass volume concentration of the sodium salt is 0.05g/L-1 g/L.
8. The eluent according to claim 5, wherein the potassium salt is selected from one or more of potassium carbonate, potassium chloride, potassium sulfate, potassium borate; the concentration of the potassium salt is 0.05g/L-1 g/L.
9. Use of an eluent according to any one of claims 5-8 for remediation of petroleum hydrocarbon contaminated soil.
10. Use according to claim 9, wherein the remediation step of the petroleum hydrocarbon contaminated soil comprises:
spraying the eluting agent into the soil polluted by petroleum hydrocarbon, and stirring for 5-20 min;
standing for 1-5 h;
injecting water and stirring for 5-60 min;
separating the soil from the liquid, and dehydrating the separated soil.
11. Use according to claim 10, wherein the mass ratio of the eluent to the petroleum hydrocarbon contaminated soil is 5: 1.
12. use according to claim 10 or 11, characterized in that the soil and the liquid are separated by centrifugation at a speed of 500-5000 rpm; the centrifugal separation time is 3min-30 min.
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| CN113174265A (en) * | 2021-04-20 | 2021-07-27 | 周子诚 | Composite heavy metal contaminated soil remediation agent and preparation method thereof |
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