CN101850358B - Method for restoring organochlorine contaminated soil - Google Patents
Method for restoring organochlorine contaminated soil Download PDFInfo
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- CN101850358B CN101850358B CN2010101995555A CN201010199555A CN101850358B CN 101850358 B CN101850358 B CN 101850358B CN 2010101995555 A CN2010101995555 A CN 2010101995555A CN 201010199555 A CN201010199555 A CN 201010199555A CN 101850358 B CN101850358 B CN 101850358B
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- soil
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- organic chloride
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- 239000002689 soil Substances 0.000 title claims abstract description 61
- 238000000034 method Methods 0.000 title claims abstract description 29
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims abstract description 11
- GVYLCNUFSHDAAW-UHFFFAOYSA-N mirex Chemical compound ClC12C(Cl)(Cl)C3(Cl)C4(Cl)C1(Cl)C1(Cl)C2(Cl)C3(Cl)C4(Cl)C1(Cl)Cl GVYLCNUFSHDAAW-UHFFFAOYSA-N 0.000 claims abstract description 7
- LCCNCVORNKJIRZ-UHFFFAOYSA-N parathion Chemical compound CCOP(=S)(OCC)OC1=CC=C([N+]([O-])=O)C=C1 LCCNCVORNKJIRZ-UHFFFAOYSA-N 0.000 claims description 8
- 230000001105 regulatory effect Effects 0.000 claims description 2
- 230000000694 effects Effects 0.000 abstract description 10
- 238000005516 engineering process Methods 0.000 abstract description 5
- 230000002195 synergetic effect Effects 0.000 abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 5
- YVGGHNCTFXOJCH-UHFFFAOYSA-N DDT Chemical compound C1=CC(Cl)=CC=C1C(C(Cl)(Cl)Cl)C1=CC=C(Cl)C=C1 YVGGHNCTFXOJCH-UHFFFAOYSA-N 0.000 abstract description 3
- 230000007613 environmental effect Effects 0.000 abstract description 3
- 239000003344 environmental pollutant Substances 0.000 abstract description 2
- 231100000719 pollutant Toxicity 0.000 abstract description 2
- 230000035484 reaction time Effects 0.000 abstract description 2
- BIWJNBZANLAXMG-YQELWRJZSA-N chloordaan Chemical compound ClC1=C(Cl)[C@@]2(Cl)C3CC(Cl)C(Cl)C3[C@]1(Cl)C2(Cl)Cl BIWJNBZANLAXMG-YQELWRJZSA-N 0.000 abstract 1
- 230000000593 degrading effect Effects 0.000 abstract 1
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 9
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 6
- 239000012259 ether extract Substances 0.000 description 5
- 239000003208 petroleum Substances 0.000 description 5
- 238000012545 processing Methods 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- 238000002604 ultrasonography Methods 0.000 description 5
- 230000015556 catabolic process Effects 0.000 description 4
- 238000006731 degradation reaction Methods 0.000 description 4
- 239000000284 extract Substances 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 238000011953 bioanalysis Methods 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- WBZKQQHYRPRKNJ-UHFFFAOYSA-L disulfite Chemical compound [O-]S(=O)S([O-])(=O)=O WBZKQQHYRPRKNJ-UHFFFAOYSA-L 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 239000005416 organic matter Substances 0.000 description 3
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 2
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 238000003795 desorption Methods 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000002386 leaching Methods 0.000 description 2
- 239000003993 organochlorine pesticide Substances 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 238000005067 remediation Methods 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000006298 dechlorination reaction Methods 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 230000005264 electron capture Effects 0.000 description 1
- 238000004710 electron pair approximation Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 238000011010 flushing procedure Methods 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 239000000852 hydrogen donor Substances 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000006210 lotion Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 238000013022 venting Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- JLYXXMFPNIAWKQ-UHFFFAOYSA-N γ Benzene hexachloride Chemical compound ClC1C(Cl)C(Cl)C(Cl)C(Cl)C1Cl JLYXXMFPNIAWKQ-UHFFFAOYSA-N 0.000 description 1
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- Processing Of Solid Wastes (AREA)
Abstract
The invention belongs to the field of polluted soil restoration, and discloses a method for restoring high-concentration organochlorine polluted soil by a microwave and ultrasonic synergistic technology, which comprises the step of treating organochlorine polluted soil with a certain water content under the irradiation conditions of microwaves and ultrasonic waves, wherein the microwave frequency is 300MHz-300GHz, the power is 0.8kW-20kW, the ultrasonic frequency is 20kHz-100kHz, the power is 100W-5kW, and the irradiation time is 3min-120 min. The organic chloride is mainly DDT, chlordane, mirex and the like. The method mainly utilizes the cavitation effect of ultrasonic waves and the heat effect and non-heat effect of microwaves to degrade organic chloride pollutants in the soil, does not damage the basic structure and the properties of the soil while efficiently degrading the organic chloride in the soil, has short reaction time, good treatment effect and no secondary pollution, and has obvious economic effect and environmental effect.
Description
Technical field
The invention belongs to the soil remediation technical field, be specifically related to contain the reparation of high concentration soil polluted by organic chloride, especially relate to a kind of method of microwave ultrasound coordination technique remedying soil polluted by organic chloride.
Background technology
Along with the process of honouring an agreement of China's industrialization and urbanization development and " Stockholm international convention ", occurred large quantities of closing in recent years and moved or waited to close the organo-chlorine pesticide manufacturing enterprise of resettlement.According to incompletely statistics, the whole nation only organo-chlorine pesticide (DDT, BHC, Niran, mirex etc.) contaminated site just have hundreds of.These places are polluted extremely heavy, and the pollutant levels total amount is mostly more than 200mg/kg.And function conversion and secondary development all are badly in need of in present most of place.The contaminated soil in these places becomes " Chemical Time Bomb ", and serious threat health and Environmental security are the current soil environment problems that presses for solution.
Existing contaminated soil recovery technique mainly contains physics method, chemical method and bioanalysis, wherein studies more have chemical leaching method, electric driving method, thermal desorption method and bioanalysis.The chemical leaching method is easy to operate, but strict to soil types, causes secondary pollution simultaneously easily; Electric driving method is easy and simple to handle, and is little to influences such as present landscape, buildings, but the processing time is longer, from several days and even several years, can cause the variation of soil pH after the anode and cathode electrolyte electrolysis simultaneously, influences soil ecology; The thermal desorption method is generally better to the stronger mass treatment effect of volatility, but does not have effect substantially for the organic matter of difficulty volatilization; The bioanalysis processing cost is low, be applicable to large-area soil remediation, but processing speed is slow, the cycle is long, generally is only applicable to handle the low concentration contaminated soil, and strict to soil environment, otherwise effective technique can efficiently be repaired the high concentration soil polluted by organic chloride so also do not have economy at present.
Summary of the invention
The objective of the invention is the defective that exists in the present heavy organic polluted soil recovery technique, and a kind of method of repairing the high concentration soil polluted by organic chloride is provided.
Technical scheme of the present invention is: a kind of method of remedying soil polluted by organic chloride, and its concrete steps are as follows:
1, regulating the soil quality moisture content is 5%-60%;
2, open microwave and supersonic generator simultaneously soil is carried out irradiation, wherein microwave frequency is 300MHz-300GHz, and power is 0.8kW-20kW, and supersonic frequency is 20kHz-100kHz, and power is 100W-5kW;
3, finish reparation behind the irradiation 3min-30min.
Organochlorine described in the present invention is meant any one or a few in DDT, Niran and the mirex.
Beneficial effect:
1. present technique is applicable to the reparation of high concentration (30mg/kg-2000mg/kg) soil polluted by organic chloride, and repairing effect is good, non-secondary pollution, economic security.
2. employing microwave technology, obvious to the organochlorine treatment effect, and also microwave can accelerate the speed of chemical reaction greatly, and the reaction time is significantly shortened.
3. microwave technology to the polar organic matter treatment effect better and speed characteristics faster, combine the characteristics of ultrasonic technique to the basic non-selectivity of organic matter, utilize microwave technology to make the polarity larger molecular organics be degraded to small organic molecule, utilize ultrasonic technique that it is thoroughly degraded simultaneously.
4. the present technique easy operating only needs the simple preliminary treatment of contaminated soil process is carried out microwave and ultrasonic irradiation to it then, gets final product behind the reaction certain hour.
5. efficient height, the cost of present technique removal organochlorine are low, speed is fast, need not outer adding medicine, and the hydrogen donor of dechlorination reaction is the water that contains in the soil, non-secondary pollution, safety and environmental protection.
The specific embodiment
Detection method
The detection method of DDT, Niran and mirex all adopts EPA Method 8081B gas chromatography in the soil.
Instrument and equipment:
Experiment needs through distillation again with acetone, benzinum (boiling range is 60～90 ℃), and prepares 1: 1 benzinum-acetone mixed solution; The concentrated sulfuric acid is pure for analyzing; Anhydrous sodium sulfate toasts 4h in 300 ℃ of baking ovens, preparation 20g/L metabisulfite solution, and residue is placed in the drier standby.
Be furnished with Tianjin, island GC-2010 gas chromatograph of ECD, chromatographic column is the RTX-1701 capillary column.
Detect:
1, extract: accurately take by weighing 10.0g soil and place small beaker, adding distil water 1mL, diatomite 2g, fully mixing nondestructively moves in the filtration paper cylinder, upper cap a slice filter paper, filtration paper cylinder is packed in the cable type extractor according, add 50mL benzinum-acetone (1: 1), soak behind the soil sample 12h on 75～95 ℃ of thermostat water baths heating with 30mL and extract 4h, the each backflow 4 times～6 times, after cooling, extract is moved in the waste liquid funnel of 300mL, divide three flushing extractors and flask with the 10mL benzinum, washing lotion is incorporated in the separatory leakage, add the 50mL metabisulfite solution, vibration 1min is behind the standing demix, discard lower floor's aqueous acetone solution, it is to be clean to stay petroleum ether extract.
2, purify (concentrated sulfuric acid purification method): 1/10th of adding petroleum ether extract volume the concentrated sulfuric acid in separatory funnel, vibration 1min, behind the standing demix, discard sulfuric acid layer and (note: in the concentrated sulfuric acid purification process, prevent the heating blast, after adding the concentrated sulfuric acid, begin slowly jolting, constantly venting, and then very fast jolting), repeat for several times by above-mentioned steps, end when transparent until the petroleum ether extract two-phase interface that adds clear all being.In the petroleum ether extract that discards sulfuric acid layer, add the metabisulfite solution of its volume about general then.Inferior surplus the jolting ten.Treat to discard water layer behind its standing demix.So be repeated to and end (general 2 times～4 times) when extract becomes neutral, petroleum ether extract is again through being equipped with the tubular funnel dehydration of a small amount of anhydrous sodium sulfate, constant volume in the volumetric flask of packing into.
3, gas Chromatographic Determination: use the gas chromatograph of being furnished with electron capture detector to detect, testing conditions is as follows:
Column temperature: 140 ℃, keep 2min; 10 ℃/min rises to 200 ℃; 5 ℃/min rises to 265 ℃
Carrier gas: helium, flow velocity 1.5mL/min
Injection port: split sampling 0.8 μ L
Split ratio: 1: 35
Injector temperature: 250 ℃
Detector temperature: 300 ℃
Embodiment 1
Fetch soil at contaminated site, the quality moisture content of soil sample is 5%-18%, behind the soil sample mixing, detecting its quality moisture content is 13%, and DDT concentration is 50.3mg/kg, satisfies the described suitable treatment condition of this patent, directly it is carried out the microwave ultrasound Synergistic degradation, treatment step is as follows:
1, the quality moisture content of processing soil sample is 13%;
2, open microwave and supersonic generator simultaneously soil is carried out irradiation, microwave frequency 2450MHz, power are 1.5kW, and supersonic frequency is 20kHz, and power is 400W;
3, exposure time is 5min.
Soil after handling is detected, and testing result shows that the concentration of DDT in the soil is 3.2mg/kg, and clearance reaches 93.6%.
Embodiment 2
The contaminated site scene is detected through on-site soil is taken a sample, and the quality moisture content of soil sample is 10%-20%, DDT concentration is 310mg/kg-350mg/kg, satisfy the described suitable treatment condition of this patent, directly it is carried out the microwave ultrasound Synergistic degradation at the contaminated site scene, treatment step is as follows:
1, the quality moisture content of processing soil sample is 10%～20%;
2, open microwave and supersonic generator simultaneously soil is carried out irradiation, microwave frequency 2450MHz, power are 5kW, and supersonic frequency is 20kHz, and power is 4kW;
3, exposure time is 15min.
Soil sample after handling is detected, and testing result shows that the concentration of DDT in the soil is 4.5mg/kg～9.6mg/kg, and average removal rate is more than 95%.
Embodiment 3
Fetch soil at contaminated site, its quality moisture content is 20%-35%, behind the soil sample mixing, detecting its quality moisture content is 31%, and Niran concentration is 230.5mg/kg by analysis, satisfies the described suitable treatment condition of this patent, it is carried out the microwave ultrasound Synergistic degradation, and treatment step is as follows:
1, the quality moisture content of soil sample is 31%;
2, open microwave and supersonic generator simultaneously soil is carried out irradiation, microwave frequency 915MHz, power are 10kW, and supersonic frequency is 60kHz, and power is 1kW;
3, exposure time is 10min.
Soil after handling is detected, and testing result shows that the concentration of Niran in the soil is 15.9mg/kg, and clearance reaches 93.1%.
Embodiment 4
Fetch soil at contaminated site, soil sample is composite pollution by analysis, its quality moisture content is 40%-55%, behind the soil sample mixing, detecting its quality moisture content is 43%, and wherein Niran concentration is 180.5mg/kg, mirex concentration is 500.3mg/kg, satisfy the described suitable treatment condition of this patent, it is carried out the microwave ultrasound Synergistic degradation, treatment step is as follows
1, the soil quality moisture content is 43%;
2, open microwave and supersonic generator simultaneously soil is carried out irradiation, microwave frequency 915MHz, power are 20kW, and supersonic frequency is 40kHz, and power is 4kW;
3, exposure time is 25min.
Soil after handling is detected, and testing result shows that Niran concentration is 13.4mg/kg in the soil, and clearance reaches 92.6%, and the concentration of mirex is 55.5mg/kg, and clearance reaches 88.9%.
Claims (2)
1. the method for a remedying soil polluted by organic chloride, its concrete steps are as follows:
A. the quality moisture content of regulating soil is 5%-60%;
B. open microwave and supersonic generator simultaneously soil is carried out irradiation, microwave frequency is 300MHz-300GHz, and power is 0.8kW-20kW; Supersonic frequency is 20kHz-100kHz, and power is 100W-5kW;
C. finish reparation behind the irradiation 3min-30min.
2. method according to claim 1 is characterized in that described organochlorine is at least a kind of in DDT, Niran and the mirex.
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| CN2010101995555A CN101850358B (en) | 2010-06-13 | 2010-06-13 | Method for restoring organochlorine contaminated soil |
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| CN2010101995555A CN101850358B (en) | 2010-06-13 | 2010-06-13 | Method for restoring organochlorine contaminated soil |
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| CN101850358B true CN101850358B (en) | 2011-11-16 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106583440A (en) * | 2016-12-22 | 2017-04-26 | 常州大学 | Method for synergistically remediating soil contaminated by organo-chlorine pesticide through nanoscale zero-valent iron/calcium peroxide |
| CN106583441A (en) * | 2016-12-22 | 2017-04-26 | 常州大学 | Method for recovery of organic chloride-polluted soil through ultrasonic intensified potassium ferrate/hydrogen peroxide |
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| CN102225424A (en) * | 2011-04-08 | 2011-10-26 | 南京农业大学 | Apparatus for eluting and restoring contaminated soil of site with integration of stirring, ultrasounds and microwaves |
| CN103272831A (en) * | 2013-03-28 | 2013-09-04 | 南京工业大学 | Device and process for integrated catalytic oxidation remediation of heavy organochlorine contaminated soil |
| CN104475439B (en) * | 2014-12-09 | 2016-08-24 | 江苏盖亚环境工程有限公司 | The restorative procedure of Niran contaminated soil |
| CN104785516B (en) * | 2015-05-18 | 2018-02-02 | 东北林业大学 | The method that ultrasonic wave and surfactant joint repair DDTs contaminated soils |
| CN105457996B (en) * | 2015-12-18 | 2018-04-06 | 广东工业大学 | A kind of method of microwave cooperating SODIUM PERCARBONATE renovation of organic pollution place soil |
| CN105689382B (en) * | 2016-01-26 | 2018-10-02 | 清华大学 | The in-situ remediation system of organic polluted soil |
| CN111408613B (en) * | 2020-03-27 | 2022-06-10 | 北京石油化工学院 | Method and system for performing microwave heat treatment on polluted soil by bidirectional coupling adjustable power |
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| CN1698984A (en) * | 2004-05-21 | 2005-11-23 | 张松 | Microwave depolymerization equipment for medical refuse treatment |
| CN1850371A (en) * | 2006-06-02 | 2006-10-25 | 清华大学 | Micro-wave heating desorption/alkyl catalytic decomposition treatment method for polychlorinated biphenyl in soil |
| CN101461990A (en) * | 2009-01-15 | 2009-06-24 | 北京师范大学 | Method for analyzing and processing persistent organic pollutants by microwave assisted base catalysis |
| CN101486520B (en) * | 2009-02-26 | 2010-09-22 | 重庆大学 | Process for treating heavy metal wastewater |
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2010
- 2010-06-13 CN CN2010101995555A patent/CN101850358B/en active Active
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106583440A (en) * | 2016-12-22 | 2017-04-26 | 常州大学 | Method for synergistically remediating soil contaminated by organo-chlorine pesticide through nanoscale zero-valent iron/calcium peroxide |
| CN106583441A (en) * | 2016-12-22 | 2017-04-26 | 常州大学 | Method for recovery of organic chloride-polluted soil through ultrasonic intensified potassium ferrate/hydrogen peroxide |
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Effective date of registration: 20210225 Address after: 210043 Building 8, Zhicheng Park, 6 Zhida Road, Jiangbei new district, Nanjing City, Jiangsu Province Patentee after: NJTECH ENVIRONMENT TECHNOLOGY Co.,Ltd. Address before: 210009 No. 200, Zhongshan North Road, Jiangsu, Nanjing Patentee before: Nanjing Tech University |