CN112694896A - Foam composition for removing heavy-phase organic pollutants in soil and preparation method thereof - Google Patents
Foam composition for removing heavy-phase organic pollutants in soil and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a foam composition for removing heavy-phase organic pollutants in soil and a preparation method thereof. The foam composition comprises: the composite material comprises, by weight, 1 part of sodium fatty acid methyl ester sulfonate, 0.1-50 parts of long-chain nitrogen-containing compound and 0.1-50 parts of nano-particles; the long-chain nitrogen-containing compound has the following structural formula:
Description
Technical Field
The invention relates to the technical field of soil remediation, in particular to a foam composition for removing heavy-phase organic pollutants in soil and a preparation method thereof.
Background
Along with the migration and reconstruction of a large number of industrial fields, the organic matter pollution of soil is concerned, and the soil remediation is more and more emphasized. The sources of organic pollutants in soil are: the leakage, leakage and discharge of three wastes in the production process of organic chemicals inevitably cause high residue in the surrounding soil; in addition, contamination can occur during the distribution and use of organic chemicals, such as pesticide abuse, improper disposal of waste, and the like. Among the many contaminants, soil contamination by non-aqueous phase liquid contaminants (NAPLs) is particularly prominent, and NAPLs can be classified into light phase liquid contaminants LNAPL (e.g., petroleum hydrocarbon contaminants) and heavy phase liquid contaminants DNAPL (e.g., polychlorinated organics) depending on their specific gravity from water. NAPLs can be bound by the formation pore media for long periods of time, thus becoming a persistent source of contamination.
Aiming at soil organic pollutants, the soil remediation technology can be divided into an in-situ remediation technology and an ex-situ remediation technology according to remediation positions, the in-situ remediation technology is more economical, the ex-situ remediation technology has lower environmental risk and easier control of treatment effect, but the treatment range is small; the operation principle can be divided into physical, chemical and biological repair technologies. The physical remediation technology has low cost and strong operability, but consumes energy, destroys the original soil structure and ecosystem, and is not suitable for large-scale application. The chemical remediation technology mainly comprises soil leaching, chemical oxidation-reduction technology and the like, and the technologies have good remediation effects on the soil with small area and heavy pollution, but have unobvious remediation effects on the soil with poor permeability, and have potential hazards of causing secondary pollution. The bioremediation technology is a relatively environment-friendly remediation technology, causes little damage to soil, but has long remediation time and limited number of applicable pollutants.
The special amphiphilic structure of the surfactant can reduce the interfacial tension and increase the solubility of an organic phase at a lower concentration, so that organic pollutants in a low-permeability area can be removed more easily; the surfactant has permeability selectivity after generating foam, and the swept volume is enlarged, so that organic matters in soil pores with different permeability can be removed as a result of the two functions.
Report on the removal of pentachlorophenol from soil by foaming with an alkylphenol ethoxylate Triton X-1001% reported in the literature "relocation with surfactant foam of PCP stabilized soil", since Triton X-100 is a weaker foaming agent, with only 85% removal of pentachlorophenol.
Disclosure of Invention
In order to solve the problems that organic pollutants are retained in pores of heterogeneous soil and are difficult to remove and secondary pollution is easily caused in the treatment process in the prior art, the foam composition for removing the heavy-phase organic pollutants in the soil and the preparation method are provided. The foam composition can form good foam, is green and easy to degrade, and does not cause secondary pollution.
It is an object of the present invention to provide a foam composition for removing heavy phase organic contaminants from soil.
The foam composition comprises:
the composite material comprises, by weight, 1 part of sodium fatty acid methyl ester sulfonate, 0.1-50 parts of long-chain nitrogen-containing compound and 0.1-50 parts of nano-particles;
the structural formula of the fatty acid methyl ester sodium sulfonate is shown as follows,
r is C10～C26An aliphatic hydrocarbon group of (1); may contain a group such as an acyl group, a carbonyl group, an ether group, a hydroxyl group, etc., may contain a saturated carbon chain or an unsaturated carbon chain, and R is preferably R1The preferred embodiment of (a) is a saturated unsaturated alkyl group; more preferably C10～C20Saturated unsaturated alkyl groups of (a);
the long-chain nitrogen-containing compound has the following structural formula:
wherein the content of the first and second substances,
R1is C10～C26Aliphatic hydrocarbon groups or aromatic hydrocarbon groups of (1); preferably C10～C20Aliphatic hydrocarbon groups or aromatic hydrocarbon groups of (1);
R2is C1～C5Alkylene of (3), preferably C2H4Or C3H6；
R3、R4Is C1～C5Alkyl of (C)2H5O or C3H7One of O;
R5is C1～C5Any one of the alkylene group and the substituted alkylene group of (1);
m is an integer of 1 to 3, preferably an integer of 1 to 2;
y is selected from anionic groups which render the molecule shown electrically neutral; preferably selected from-COO-、-SO3 -、-HPO4 -At least one of (1).
The nanoparticles are preferably nanosilica; preferably, the particle size is less than or equal to 600 nm.
Preferably, the weight ratio of the fatty acid methyl ester sodium sulfonate to the long-chain nitrogen-containing compound to the nano particles is 1: 0.2-10.
The invention also aims to provide a preparation method of the foaming agent composition for removing heavy-phase organic pollutants in soil.
The method comprises the following steps:
the components are mixed according to the dosage, water is added, and the foam composition for removing the heavy-phase organic pollutants in the soil is prepared after the components are stirred to be completely dissolved.
Among them, water is preferably added to prepare a 0.5 to 5 wt% solution.
The key active ingredients of the foaming agent are sodium fatty acid methyl ester sulfonate, long-chain nitrogen-containing compounds and nano particles, and the person skilled in the art knows that the foaming agent can be supplied in various forms for transportation and storage or on-site use, such as non-aqueous solid form, aqueous paste form or aqueous solution form; the water solution form comprises a form of preparing a concentrated solution by using water and a form of directly preparing a foaming agent with concentration required by on-site oil displacement; the water is not particularly required, and can be deionized water or water containing inorganic minerals, and the water containing the inorganic minerals can be tap water or formation water.
The sodium fatty acid methyl ester sulfonate and the long-chain nitrogen-containing compound in the composition are green and easily degradable surfactants, so that secondary pollution to the stratum is avoided, and the nanoparticles are selected from inorganic substances contained in the stratum and cannot cause secondary pollution. The electrostatic interaction between the long-chain nitrogen-containing compound and the nano-particles and the electrostatic interaction between the sodium fatty acid methyl ester sulfonate and the long-chain nitrogen-containing compound enhance the adsorption capacity and the strength of a liquid film after the system is mixed with gas to form foam, and expand the swept volume aiming at the heterogeneous soil.
The composition, 1.0PV foaming agent aqueous solution, can remove 95% of organic residues after forming foam with gas, and achieves better technical effect.
Detailed Description
The present invention will be further described with reference to the following examples.
While the present invention will be described in detail with reference to the following examples, it should be understood that the following examples are illustrative of the present invention and are not to be construed as limiting the scope of the present invention.
The long-chain nitrogen-containing compound in the examples is self-made, and other raw materials are all commercial products.
The nanoparticles used in the examples are all silica; the nanoparticle diameters in the examples were 10nm and 50 nm.
Example 1
Preparation of long-chain nitrogen-containing compound:
adding 200 g (1.0 mol) of lauric acid, 149 g (1.25 mol) of thionyl chloride and 3 g of DMF into a four-necked flask equipped with a sealed mechanical stirrer, a thermometer, a condenser tube and the like, reacting at 90 ℃ for 3 hours, and then distilling off excess thionyl chloride under reduced pressure to obtainLauroyl chloride. When the temperature is reduced to 60 ℃, 70 g of toluene is added, after uniform stirring, a mixed solution consisting of 131 g (1.0 mol) of dipropylene triamine and 99.0 g (1.25 mol) of pyridine is slowly dripped, the temperature is controlled to be less than 60 ℃, and the temperature is raised to 85 ℃ after dripping for 2 hours. Cooling, filtering, recrystallizing the crude product with ethanol, and vacuum drying to obtain white powdery solid C11H23CO(NHC3H6)2NH2The yield thereof was found to be 91%.
157 g of C are introduced into a reactor equipped with a condensing device, a stirring device and a gas disperser11H23CO(NHC3H6)2NH2(0.5 mol), heating to 80-90 ℃, starting a vacuum system, dehydrating for 1 hour under high vacuum, then purging for 3-4 times by using nitrogen to remove air in the system, adjusting the reaction temperature of the system to 130 ℃, slowly introducing 44 g of ethylene oxide (1.0 mol), and controlling the pressure to be less than 0.60MPa to carry out alkoxylation; after the reaction is finished, purging the system by nitrogen to remove unreacted ethylene oxide, cooling, neutralizing, decoloring, filtering and dehydrating to obtain C11H23CO(NHC3H6)2N(C2H4O)2The yield thereof was found to be 80%.
120 g of C was placed in a four-necked round-bottomed flask equipped with a reflux condenser, a thermometer and a stirrer11H23CO(NHC3H6)2N(C2H4O)2(0.3 mol) and 100 g of isopropanol, heating to 70 ℃ under stirring, slowly dropwise adding 313 g (0.4 mol) of 25% sodium 3-chloro-2-hydroxypropanesulfonate by using a dropping funnel, reacting for 10 hours at 90 ℃ after the dropwise addition is finished, and treating to obtain C11H23CO(NHC3H6)2N(C2H4O)2CH2CH(OH)CH2SO3The yield was 83 wt%.
Preparation of composition HF-1, preparation procedure:
weighing 2 g of sodium methyl dodecanoate sulfonate at normal temperature and normal pressure, and adding a long-chain nitrogen-containing compound (C)11H23CO(NHC3H6)2N(C2H4O)2CH2CH(OH)CH2SO3)0.4 g of the foaming agent composition HF-1 is obtained by adding enough local tap water to 150 g of the nanoparticle solution (containing 0.6 g of the nanoparticles) into a reaction kettle, preparing the solution with the weight percent of 2 percent, and fully stirring for 30min until the solution is completely dissolved.
Example 2
Preparation of long-chain nitrogen-containing compound:
in a four-necked flask equipped with a sealed mechanical stirrer, a thermometer, a condenser and the like, 256 g (1.0 mol) of hexadecanoic acid, 149 g (1.25 mol) of thionyl chloride and 3 g of DMF were charged, reacted at 90 ℃ for 3 hours, and then excess thionyl chloride was distilled off under reduced pressure to obtain hexadecanoyl chloride. When the temperature is reduced to 60 ℃, 70 g of toluene is added, after uniform stirring, a mixed solution consisting of 102 g (1.0 mol) of N, N-dimethyl-1, 3-propane diamine and 99.0 g (1.25 mol) of pyridine is slowly dropped, the temperature is controlled to be less than 60 ℃, and the temperature is raised to 85 ℃ after dropping for 2 hours. Cooling, filtering, recrystallizing the crude product with ethanol, and vacuum drying to obtain white powdery solid C15H31CONHC3H6N(CH3)2The yield thereof was found to be 95%.
170 g of C was placed in a four-necked round-bottomed flask equipped with a reflux condenser, a thermometer and a stirrer15H31CONHC3H6N(CH3)2(0.5 mol) and 150 g of isopropanol, heating to 70 ℃ under stirring, slowly dropwise adding 350 g (0.6 mol) of 25% sodium chlorobutyrate by using a dropping funnel, reacting at 90 ℃ for 10 hours after the dropwise adding is finished, and treating to obtain C15H31CONHC3H6N(CH3)2C3H6COO in a yield of 89 wt%. Preparation of composition HF-2, preparation procedure:
weighing 1 g of sodium methyl hexadecanoate sulfonate at normal temperature and normal pressure, and adding long-chain nitrogen-containing compound (C)15H31CONHC3H6N(CH3)2C3H6COO)1.2 g into a reaction kettle, a nanoparticle solution (containing 0.8 g of nanoparticles), andadding enough local tap water to 300 g to prepare a 1 wt% solution, and fully stirring for 30min until the solution is completely dissolved to obtain the foaming agent composition HF-2.
Example 3
Preparation of long-chain nitrogen-containing compound:
the preparation process is the same as that of example 1 except that the raw materials (pentadecanoic acid, propylenediamine, propylene oxide, sodium chlorobutyrate) are different from those of example 1, and the long-chain nitrogen-containing compound (C) is obtained14H29CONHC3H6N(C3H7O)2C3H6COO)；
Preparation of composition HF-3, preparation procedure:
weighing 2 g of sodium methyl eicosanoate sulfonate at normal temperature and normal pressure, and adding the long-chain nitrogen-containing compound (C)14H29CONHC3H6N(C3H7O)2C3H6COO)0.5 g into a reaction kettle, adding enough local tap water to 60 g of the nanoparticle solution (containing 0.5 g of nanoparticles), preparing into a solution with the weight percent of 5%, and fully stirring for 30min until the solution is completely dissolved, thus obtaining the foaming agent composition HF-3.
Example 4
Preparation of long-chain nitrogen-containing compound:
the same example 2, except that the raw materials were different (tetradecylbenzoic acid, N' -di-N-propylethylenediamine, sodium chloropropanesulfonate), was followed by the same procedure as in example 2 to obtain a long-chain nitrogen-containing compound (C)20H33CONHC2H4N(C3H7)2C3H6SO3)；
Preparation of composition HF-4, preparation procedure:
at normal temperature and pressure, 0.2 g of sodium methyl tallate sulfonate is weighed, and then long-chain nitrogen-containing compound (C) is added into the sodium methyl tallate sulfonate20H33CONHC2H4N(C3H7)2C3H6SO3)2 g into the reactor, the nanoparticle solution (containing 0.2 g of nanoparticles) was added with sufficient amount of native tap waterAnd (3) adding water to 120 g to prepare a 2 wt% solution, and fully stirring for 30min until the solution is completely dissolved to obtain the foaming agent composition HF-4.
Example 5
Preparation of long-chain nitrogen-containing compound:
the preparation process of the same example 1 except for the raw materials (pentadecanoic acid, triethylene tetramine, propylene oxide, sodium chloropropanesulfonate) as in example 1 gave a long-chain nitrogen-containing compound (C)14H29CO(NHC2H4)3N(C3H7O)2C3H6SO3)；
Preparation of composition HF-5, preparation procedure:
weighing 2 g of sodium methyl dodecanoate sulfonate at normal temperature and normal pressure, and adding a long-chain nitrogen-containing compound (C)14H29CO(NHC2H4)3N(C3H7O)2C3H6SO3)0.4 g of the foaming agent composition HF-5 is obtained by adding enough local tap water to 150 g of the nanoparticle solution (containing 0.6 g of the nanoparticles) into a reaction kettle, preparing the solution with the weight percent of 2 percent, and fully stirring for 30min until the solution is completely dissolved.
Example 6
Preparation of long-chain nitrogen-containing compound:
same as example 2
Preparation of composition HF-6, preparation procedure:
at normal temperature and normal pressure, 1 g of sodium methyl hexacosanoate sulfonate is weighed, and then a long-chain nitrogen-containing compound (C) is added into the sodium methyl hexacosanoate sulfonate15H31CONHC3H6N(CH3)2C3H6COO)1.2 g into a reaction kettle, adding enough local tap water into the nanoparticle solution (containing 0.8 g of nanoparticles) to 300 g to prepare a 1 wt% solution, and fully stirring for 30min until the solution is completely dissolved to obtain the foaming agent composition HF-6.
Example 7
Preparation of long-chain nitrogen-containing compound:
the same as in example 2.
Preparation of composition HF-7, preparation procedure:
0.1 g of sodium methyl hexadecanoate sulfonate is weighed at normal temperature and normal pressure, and then the long-chain nitrogen-containing compound (C) is added into the sodium methyl hexadecanoate sulfonate15H31CONHC3H6N(CH3)2C3H6COO)5 g into a reaction kettle, adding sufficient local tap water into the nanoparticle solution (containing 0.5 g of nanoparticles) to 560 g to prepare a 1 wt% solution, and fully stirring for 30min until the solution is completely dissolved to obtain the foaming agent composition HF-7.
Example 8
Preparation of long-chain nitrogen-containing compound:
the same as in example 2.
Preparation of composition HF-8, preparation procedure:
0.1 g of sodium methyl hexadecanoate sulfonate is weighed at normal temperature and normal pressure, and then the long-chain nitrogen-containing compound (C) is added into the sodium methyl hexadecanoate sulfonate15H31CONHC3H6N(CH3)2C3H6COO)1 g into a reaction kettle, adding enough local tap water into the nanoparticle solution (containing 5 g of nanoparticles) to 305 g to prepare a 2 wt% solution, and fully stirring for 30min until the solution is completely dissolved to obtain the foaming agent composition HF-8.
Example 9
Filling a plane sand filling model with different upper and lower permeability rates, wherein the upper layer permeability rate is 5000mD, the lower layer permeability rate is 50mD, after saturated water is obtained, displacing the mixed pollutant with 1: 1 of trichloroethylene and tetrachloroethylene until the pollutant is saturated, injecting the composition HF-1 and nitrogen in the embodiment 1 for displacement, and recording the displacement of the pollutant by the injection amount of the foaming agent composition of 0.5pV and 1.0 pV; then injecting water until no surfactant and gas are displaced, then displacing the mixed pollutants until the pollutants are saturated, then injecting the composition HF-2 and nitrogen in the embodiment 2 for displacement, and recording the injection amount of the foaming agent composition, namely 0.5pV and 1.0pV for displacement of the pollutants; then injecting water until no surfactant and gas are displaced, then displacing the mixed pollutants until the pollutants are saturated, then injecting the composition HF-3 and nitrogen in the embodiment 3 for displacement, and recording the injection amount of the foaming agent composition, namely 0.5pV and 1.0pV for displacement of the pollutants; by analogy, the amount of contaminant displaced by the compositions HF-4- -HF-8 of examples 4-8 was recorded and the results are shown in Table 1. The volume ratio of the foam composition to nitrogen gas was 2 to 8.
Comparative example 1
Use of C synthesized in [ example 1 ]11H23CO(NHC3H6)2N(C2H4O)2CH2CH(OH)CH2Synthesis of C in SO [ example 2 ]15H31CONHC3H6N(CH3)2C3H6COO, C synthesized in [ example 3 ]14H29CONHC3H6N(C3H7O)2C3H6COO, C synthesized in [ example 4 ]20H33CONHC2H4N(C3H7)2C3H6SO3C synthesized in [ example 5 ]14H29CO(NHC2H4)3N(C3H7O)2C3H6SO3The foam compositions were prepared as single agents, without the addition of subsequent components, and the results of the contaminant displacement test were as described in example 9, and are shown in table 2.
Comparative example 2
A foam composition was prepared using sodium methyl dodecanoate sulfonate in [ example 1 ], sodium methyl hexadecanoate sulfonate in [ example 2 ], sodium methyl eicosanoate sulfonate in [ example 3 ], sodium methyl taurate in [ example 4 ] as the single agent, without adding subsequent components, and a contaminant displacement test was performed as in [ example 9 ], with the results shown in table 3.
Comparative example 3
Using 2% nanoparticles, a contaminant displacement test was performed as in example 9, with 1.0pV displacing only 20% of the trichloroethylene and tetrachloroethylene 1 to 1 mixed contaminant.
As can be seen from the data in tables 1 to 3, the foam agent composition prepared by the method has very remarkable displacement effect, and the foam agent aqueous solution with the pore volume of 1.0PV can remove more than 95% of organic residues after forming foam with gas.
Claims (10)
1. A foam composition for removing heavy phase organic contaminants from soil, said foam composition comprising:
the composite material comprises, by weight, 1 part of sodium fatty acid methyl ester sulfonate, 0.1-50 parts of long-chain nitrogen-containing compound and 0.1-50 parts of nano-particles;
the structural formula of the fatty acid methyl ester sodium sulfonate is shown as follows,
r is C10～C26An aliphatic hydrocarbon group of (1);
the long-chain nitrogen-containing compound has the following structural formula:
wherein R is1Is C10～C26Aliphatic hydrocarbon groups or aromatic hydrocarbon groups of (1); r2Is C1～C5Alkylene of (A), R5Is C1～C5Any one of the alkylene group and the substituted alkylene group of (1); r3、R4Is C1～C5Alkyl of (C)2H5O or C3H7One of O; m is an integer from 1 to 3 and Y is selected from anionic groups which render the molecule shown electrically neutral.
2. The foam composition of claim 1, wherein:
r is C10～C20Saturated unsaturated alkyl groups of (2).
3. The foam composition of claim 1, wherein:
R1is C10～C20Aliphatic hydrocarbon groups or aromatic hydrocarbon groups.
4. The foamable composition of claim 1, wherein:
and m is an integer of 1-2.
5. The foamable composition of claim 1, wherein:
R2is C2H4Or C3H6。
6. The foamable composition of claim 1, wherein:
y is selected from-COO—、-SO3 —、-HPO4 —At least one of (1).
7. The foamable composition of claim 1, wherein:
the nano particles are nano silicon dioxide; the grain diameter is less than or equal to 600 nm.
8. The foamable composition of claim 1, wherein:
the weight ratio of the fatty acid methyl ester sodium sulfonate to the long-chain nitrogen-containing compound to the nano particles is 1 (0.2-10) to (0.2-10).
9. A process for preparing a foamable composition according to any one of claims 1 to 8, wherein the process comprises:
the components are mixed according to the dosage, water is added, and the foam composition for removing the heavy-phase organic pollutants in the soil is prepared after the components are stirred to be completely dissolved.
10. The method of claim 9, wherein:
adding water to prepare 0.5-5 wt% solution.
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| 李英: "采用低张力水基泡沫修复有机物或重金属离子污染的土壤", 《首届全球华人科学家环境论坛论文(摘要)汇编》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114247742A (en) * | 2021-12-13 | 2022-03-29 | 上海化工研究院有限公司 | Foam composite repairing material for treating peculiar smell of polluted soil and treating method |
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