CN104550221A - Eluent for a pesticide-DDT in black soil and eluting method of eluent - Google Patents
Eluent for a pesticide-DDT in black soil and eluting method of eluent Download PDFInfo
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- CN104550221A CN104550221A CN201410718549.4A CN201410718549A CN104550221A CN 104550221 A CN104550221 A CN 104550221A CN 201410718549 A CN201410718549 A CN 201410718549A CN 104550221 A CN104550221 A CN 104550221A
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Abstract
The invention discloses an eluent for a pesticide-DDT in black soil and an eluting method of the eluent. The eluent disclosed by the invention is composed of a non-ionic surfactant, an anionic surfactant, inorganic salt, an organic additive and a solvent. The specific composition of the eluent is as follows: the mass ratio of the non-ionic surfactant-twain 60 to the anionic surfactant-sodium dodecyl sulfate in the eluent is (1-3) to 1, the total concentration of the two is 3000-4000mg/L, the concentration of the inorganic salt-K2SiO3 or K2CO3 in the eluant is 1.0g/L, the concentration of the organic additive-n-propanol or n-butyl alcohol in the eluent is 1.0-2.0mol/L, and the solvent is water.
Description
Technical field
The invention belongs to soil organic contamination processing technology field, be specifically related to a kind of eluant, eluent to black earth Pesticides DDT and elution process thereof.
Background technology
In recent years, the aggravation of mankind's activity and irrational Land_use change cause the black earth being always considered to " pure land " to be faced with the crisis of environmental pollution.Especially remain a large amount of agricultural chemicals in the chemical plant in urban district and suburbs, insecticide factory's old site soil environment, and to underground water and surrounding area diffusion, bring very important threat to the healthy of local crowd and ecological environment.
Organo-chlorine pesticide DDT (DDTs) started to be widely used in control of agricultural pest in China from the fifties in last century, was still used as now the intermediate of dicofol, anti-fouling paint additive and for Disease epizootic etc.Because this compound property is stablized, be difficult to decompose at occurring in nature, in China's various places soil environment, still have higher remaining at present.Research shows, soil is to the adsorption capacity of organic pollution and soil organic matter content correlation, and in black soil of Northeast China, the content of organic matter is enriched, and strong to the absorption accumulation ability of organic pollution, residual concentration is high.Therefore, efficiently, fast the repairing and treating technology of DDTs Contaminated Phaiozem is very necessary in research and development in time.
Because the vapour pressure of DDTs is little, octanol-water partition coefficient is high, is very easily firmly adsorbed by soil particle thing, causes bioavailability poor, seriously constrains the remediation efficiency of soil.How to impel DDTs from soil significantly desorb get off, improve further its solvability in liquid phase of soil, become the key factor improving DDTs contaminated soil drip washing remediation efficiency.Soil elution recovery technique is a kind of effective chemical repair method, can by the liquid phase wash-out contaminated soil that can promote that pollutant dissolves, the pollutant be adsorbed on soil particle is made to be dissolved in liquid phase and the technology removed, in this technology energy short time fast, the soil pollution of high-efficient purification high concentration, and disposal cost is comparatively cheap, it is the soil restoring technology being considered to most potentiality at present.
In recent years, surfactant drip washing recovery technique obtains paying close attention to widely both at home and abroad, its principle is the solubilization utilizing surfactant micella, promote that the organic pollution of soil particle absorption discharges to liquid phase, improve its bioavailability, thus reach the object improving soil elution and biological prosthetic efficiency.At present, in this technology, the single surfactant of many employings carries out drip washing reparation, but research shows that single surfactant wash-out recovery technique comes with some shortcomings, and the precipitation loss as anion surfactant can reduce wash-out remediation efficiency, increases wash-out cost etc.And anion-nonionic combined surfactant has synergistic solubilization to organic pollution, and reduce the loss of single surfactant adsorption precipitation, improve the effect that wash-out is repaired.The domestic surfactant recovery technique to contaminated soil has carried out some researchs, but the implementation condition of this technology has very big-difference because of soil types, the domestic wash-out recovery technique still lacked DDTs in black soil at present.
Summary of the invention
Object of the present invention is intended to for the domestic recovery technique demand to pollution by pesticides black earth such as DDTs, provide a kind of by anion-nonionic surfactant, inorganic and organic additive is formulated, can efficient, the new soil eluant, eluent of repairing DDTs Contaminated Phaiozem fast.
To achieve these goals, the present invention adopts following technical scheme to realize:
Eluant, eluent to black earth Pesticides DDT of the present invention is by non-ionic surface active agent, anion surfactant, inorganic salts, organic additive and solvent composition; Specifically composed as follows: the mass ratio of non-ionic surfactant Tween 60 and anionic is 1 ~ 3:1, the two total concentration in eluant, eluent is 3000 ~ 4000mg/L, inorganic salts K
2siO
3or K
2cO
3in eluant, eluent, concentration is 1.0g/L, and organic additive normal propyl alcohol or n-butanol concentration in eluant, eluent is 1.0 ~ 2.0mol/L, and solvent is water.
As one of preferred technical scheme: the mass ratio of polysorbate60 and lauryl sodium sulfate is 2:1, the two total concentration in eluant, eluent is 3000mg/L, K
2cO
3the 1.0g/L that concentration is in eluant, eluent, n-butanol concentration in eluant, eluent is 2.0mol/L, and solvent is water.
As preferred technical scheme two: the mass ratio of polysorbate60 and lauryl sodium sulfate is 3:1, the two total concentration in eluant, eluent is 4000mg/L, K
2siO
3the 1.0g/L that concentration is in eluant, eluent, n-butanol concentration in eluant, eluent is 2.0mol/L, and solvent is water.
As preferred technical scheme three: the mass ratio of polysorbate60 and lauryl sodium sulfate is 3:1, the two total concentration in eluant, eluent is 4000mg/L, K
2cO
3the 1.0g/L that concentration is in eluant, eluent, normal propyl alcohol concentration in eluant, eluent is 2.0mol/L, and solvent is water.
The concrete steps of eluant, eluent of the present invention to the elution process of the black earth containing agricultural chemicals DDT are as follows:
(1) after gesarex polluted for agricultural chemicals black earth being removed stone, rhizome impurity, grinding by the soil sieve of 2mm;
(2) eluant, eluent is mixed according to the ratio of volume (ml) weight (g) than 10 ~ 15:1 with contaminated soil;
(3) mixed system is placed in constant temperature oscillator, lucifuge vibration under 150 ~ 200r/min, eluent is fully contacted with contaminated soil, eluting temperature is controlled at 25 ~ 35 DEG C, elution time is 4 ~ 8 hours, for the aging soil that the time of pollution is longer, elution time can extend to 12 ~ 24 hours;
(4) vibrate after wash-out terminates, centrifugation eluent under 4000r/min, replaces the method wash-out 1 ~ 2 hour of eluant, eluent according to step (3) by soil deionized water, backfills after the black soil natural air drying after reparation.
Compared with prior art, advantage of the present invention is:
1. the present invention is not only applicable to the wash-out reparation of DDT Contaminated Phaiozem, has good wash-out removal effect to DDD, DDE and the DBP etc. in black earth simultaneously yet, and therefore the handling object of this eluant, eluent comprises all DDTs pollutants of DDT metabolite.
2. not only stability is high, solubilising eluting power is strong for each surfactant adopted in this soil elution agent, use not by electrolyte and impact that is sour, alkali, and all the components all merchandized handling, environmental friendliness, cheap, eluant, eluent using method is simple, to equipment and horsepower requirements not high, easy to operate.
3. this soil elution agent adopts a cloudy nonionic surfactant combinations, and its character is different from single surfactant.Non-ionic surface active agent can reduce anion surfactant Krafft point, improves resistance to hard water, reduces the precipitation loss in soil; And anion surfactant can reduce the adsorption loss of non-ionic surface active agent on soil mineral, increase its valid density.The soil elution effect of the single non-ionic surface active agent of this group of surfactants composition and division in a proportion improves about 20%.
4. the inorganic salts in this soil elution agent by reducing hydrophobic organic compound interfacial tension in the liquid phase with the interaction of surfactant, can improve the dispersal ability of organic matter to aqueous phase; On the other hand by the ionic atmosphere thickness of a large amount of ion compression surface active agent ion heads of hydrolysis generation, promote micelle forma-tion, thus improve elution efficiency.Inorganic salts in this soil elution agent are K with low cost
2siO
3or K
2cO
3, the eluting rate of DDTs can be improved about 40%.It is recyclable that wash-out terminates rear most of inorganic salts, can not bring secondary pollution to soil, and K is the nutrient that soil itself has, and can improve the biologically active of soil.
5. the organic additive in this soil elution agent can reduce surfactant micella group's ordered arrangement and form the ability of hydrogen bond, thus makes micelle become loose; Organic additive easily enters micelle kernel simultaneously, micelle is swollen, is conducive to DDTs and enters in the palisade layer of expansion, increase its solubilizing amount, thus makes elution efficiency improve 10 ~ 20%.
6. last in the present invention with deionized water wash-out soil, object is to wash off the eluant compositions such as the surfactant remained in soil, to avoid eluant composition to enter into the soil after reparation as far as possible, reduces the risk of secondary pollution.
Detailed description of the invention
Below by specific embodiment, the present invention will be further elaborated; but not limiting the scope of the invention; on the basis of technical scheme of the present invention, those skilled in the art do not need to pay various amendment or distortion that creative work can make still within protection scope of the present invention.
Embodiment 1: the elute effect of low concentration DDTs POLLUTION SIMULATION soil
The composition of soil elution agent is: the mass ratio of polysorbate60 and lauryl sodium sulfate is 2:1, and the two total concentration is the K of 3000mg/L, 1.0g/L
2cO
3, the n-butanol of 2.0mol/L, solvent is water.Be dissolved in dichloromethane solvent by a certain amount of DDT, joining obtained concentration in pedotheque is the DDT simulating pollution soil sample of 10mg/kg.The DDTs accurately taking 4.0g pollutes soil sample and puts into 100ml conical flask, add the soil elution agent also fully mixing (solid-to-liquid ratio 1:10) that 40ml has prepared, after sealing, aluminium-foil paper parcel, conical flask is placed in air bath constant temperature oscillator, vibrates 4 hours with 200r/min lucifuge under 30 DEG C of conditions.Natural air drying after soil washed with de-ionized water after mud-water separation.Soil elution liquid, with the centrifugation 10min of 4000r/min, pipettes the C of supernatant by activating through methyl alcohol
18solid-phase extraction column, with 40ml hexane C
18solid-phase extraction column, collects eluent.Eluent is through anhydrous Na
2sO
4be concentrated into Rotary Evaporators near dry after dehydration, add 2ml n-hexane dissolution, the concentration of DDT in gas chromatograph for determination eluent.In this Soil Under Conditions, the clearance of DDT is 77.28%.
Embodiment 2: the elute effect of high concentration DDTs POLLUTION SIMULATION soil
The composition of soil elution agent is: the mass ratio of polysorbate60 and lauryl sodium sulfate is 3:1, and the two total concentration is the K of 4000mg/L, 1.0g/L
2cO
3, the n-butanol of 2.0mol/L, solvent is water.Be dissolved in dichloromethane solvent by a certain amount of DDT, joining obtained concentration in pedotheque is the DDT simulating pollution soil sample of 100mg/kg.The DDTs accurately taking 4.0g pollutes soil sample and puts into 100ml conical flask, add the soil elution agent also fully mixing (solid-to-liquid ratio 1:15) that 60ml has prepared, after sealing, aluminium-foil paper parcel, conical flask is placed in air bath constant temperature oscillator, vibrates 6 hours with 200r/min lucifuge under 30 DEG C of conditions.Clean again once by same method after mud-water separation, soil washed with de-ionized water natural air drying.Soil elution liquid measures the concentration of DDT in eluent by the method in embodiment 1.In this Soil Under Conditions, a wash-out clearance of DDT is 47.34%, and secondary wash-out place to go rate is 65.38%.
The elute effect of embodiment 3:DDTs contaminated site soil
The composition of soil elution agent is: the mass ratio of polysorbate60 and lauryl sodium sulfate is 3:1, and the two total concentration is the K of 4000mg/L, 1.0g/L
2siO
3, the normal propyl alcohol of 2.0mol/L, solvent is water.DDTs pollutes soil sample and adopts northeast pesticide producing enterprise old site contaminated soil, after measured, in soil, the concentration of the DDT that available n-hexane extracts is the concentration of 16.31mg/kg, DDD is 5.17mg/kg, DDE concentration is 6.94mg/kg, DDTs total concentration is 28.42mg/kg.The DDTs accurately taking 8.0g pollutes soil sample and puts into 200ml conical flask, add the soil elution agent also fully mixing (solid-to-liquid ratio 1:12.5) that 100ml has prepared, after sealing, aluminium-foil paper parcel, conical flask is placed in air bath constant temperature oscillator, vibrates 12 hours with 200r/min lucifuge under 30 DEG C of conditions.Soil washed with de-ionized water natural air drying after mud-water separation.Measure the total concentration of DDTs in eluent by the method in embodiment 1 after the mixing of soil elution liquid.In this Soil Under Conditions, the clearance of DDTs is 62.89%.
The elute effect of embodiment 4:DDTs contaminated site soil
The composition of soil elution agent is: the mass ratio of polysorbate60 and lauryl sodium sulfate is 3:1, and the two total concentration is the K of 4000mg/L, 1.0g/L
2cO
3, the normal propyl alcohol of 2.0mol/L, solvent is water.DDTs pollutes soil sample and adopts northeast pesticide producing enterprise old site contaminated soil, after measured, in soil, the concentration of the DDT that available n-hexane extracts is the concentration of 27.74mg/kg, DDD is 7.12mg/kg, DDE concentration is 13.21mg/kg, DDTs total concentration is 48.07mg/kg.The DDTs accurately taking 8.0g pollutes soil sample and puts into 200ml conical flask, add the soil elution agent also fully mixing (solid-to-liquid ratio 1:15) that 120ml has prepared, after sealing, aluminium-foil paper parcel, conical flask is placed in air bath constant temperature oscillator, vibrates 12 hours with 200r/min lucifuge under 30 DEG C of conditions.Consider that pollution history is longer, DDTs is combined with soil particle closely, the soil after wash-out is pressed again same method wash-out 1 time.Soil washed with de-ionized water natural air drying after mud-water separation.Measure the total concentration of DDTs in eluent by the method in embodiment 1 after the mixing of soil elution liquid.In this Soil Under Conditions, the clearance of DDTs is 72.91%.
Although illustrate and describe embodiments of the invention, for the ordinary skill in the art, be appreciated that and can carry out multiple change, amendment, replacement and modification to these embodiments without departing from the principles and spirit of the present invention, scope of the present invention is by claims and equivalents thereof.
Claims (5)
1. to an eluant, eluent for black earth Pesticides DDT, it is characterized in that: described eluant, eluent is by non-ionic surface active agent, anion surfactant, inorganic salts, organic additive and solvent composition; Specifically composed as follows: non-ionic surfactant Tween 60 and the anionic mass ratio in eluant, eluent is 1 ~ 3:1, the two total concentration is 3000 ~ 4000mg/L, inorganic salts K
2siO
3or K
2cO
3in eluant, eluent, concentration is 1.0g/L, and organic additive normal propyl alcohol or n-butanol concentration in eluant, eluent is 1.0 ~ 2.0mol/L, and solvent is water.
2. the eluant, eluent to black earth Pesticides DDT as claimed in claim 1, is characterized in that: the mass ratio of polysorbate60 and lauryl sodium sulfate is 2:1, and the two total concentration in eluant, eluent is 3000mg/L, K
2cO
3the 1.0g/L that concentration is in eluant, eluent, n-butanol concentration in eluant, eluent is 2.0mol/L, and solvent is water.
3. the eluant, eluent to black earth Pesticides DDT as claimed in claim 1, is characterized in that: the mass ratio of polysorbate60 and lauryl sodium sulfate is 3:1, and the two total concentration in eluant, eluent is 4000mg/L, K
2siO
3the 1.0g/L that concentration is in eluant, eluent, n-butanol concentration in eluant, eluent is 2.0mol/L, and solvent is water.
4. the eluant, eluent to black earth Pesticides DDT as claimed in claim 1, is characterized in that: the mass ratio of polysorbate60 and lauryl sodium sulfate is 3:1, and the two total concentration in eluant, eluent is 4000mg/L, K
2cO
3the 1.0g/L that concentration is in eluant, eluent, normal propyl alcohol concentration in eluant, eluent is 2.0mol/L, and solvent is water.
5. the eluant, eluent as described in any one of Claims 1 to 4, to the elution process of the black earth containing agricultural chemicals DDT, is characterized in that: the concrete steps of described method are as follows:
(1) after gesarex polluted for agricultural chemicals black earth being removed stone, rhizome impurity, grinding by the soil sieve of 2mm;
(2) eluant, eluent is mixed according to the ratio of volume (ml) weight (g) than 10 ~ 15:1 with contaminated soil;
(3) mixed system is placed in constant temperature oscillator, lucifuge vibration under 150 ~ 200r/min, eluent is fully contacted with contaminated soil, eluting temperature is controlled at 25 ~ 35 DEG C, elution time is 4 ~ 8 hours;
(4) vibrate after wash-out terminates, centrifugation eluent under 4000r/min, replaces the method wash-out 1 ~ 2 hour of eluant, eluent according to step (3) by soil deionized water, backfills after the black soil natural air drying after reparation.
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| CN201410718549.4A CN104550221A (en) | 2014-12-01 | 2014-12-01 | Eluent for a pesticide-DDT in black soil and eluting method of eluent |
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| CN104785516A (en) * | 2015-05-18 | 2015-07-22 | 东北林业大学 | Method for remediating DDTs contaminated soil by virtue of combination of ultrasonic waves and surfactants |
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| CN105903759A (en) * | 2016-04-13 | 2016-08-31 | 沈阳大学 | Method for restoring anofex-polycyclic aromatic hydrocarbon composite polluted soil by biological agent |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104785516A (en) * | 2015-05-18 | 2015-07-22 | 东北林业大学 | Method for remediating DDTs contaminated soil by virtue of combination of ultrasonic waves and surfactants |
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| CN105903759B (en) * | 2016-04-13 | 2018-10-09 | 沈阳大学 | A kind of method that biological agent repairs DDT-polycyclic aromatic hydrocarbon composite pollution soil |
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Application publication date: 20150429 |