CN101024527A - Use of modified montmorillonite as organic chlorine farm chemicals adsorbant in dewatering system - Google Patents
Use of modified montmorillonite as organic chlorine farm chemicals adsorbant in dewatering system Download PDFInfo
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- CN101024527A CN101024527A CN 200710056729 CN200710056729A CN101024527A CN 101024527 A CN101024527 A CN 101024527A CN 200710056729 CN200710056729 CN 200710056729 CN 200710056729 A CN200710056729 A CN 200710056729A CN 101024527 A CN101024527 A CN 101024527A
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- organochlorine pesticide
- pesticide
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- organic chlorine
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Abstract
The invention discloses a method to use modified montorillonite clay as process organochlorine pesticide water body adsorbent. It has very good adsorption effect to trace amount organochlorine pesticide in solution. The equal adsorption capacity is 50ug/g.
Description
Technical field
The present invention relates to the purposes of modified montmorillonoid, relate in particular to purposes in the water field of purification.
Technical background
Remove the organochlorine pesticide method at present in the aqueous systems and mainly contain absorption method, coagulant sedimentation and supercritical extraction etc.Wherein coagulant sedimentation is difficult to reach the standard of 0.1mg/L to the processing of organochlorine pesticide in the water; Because the rise of supercritical extraction technique also has the research that much utilizes supercritical technology that organochlorine pesticide in the water is removed, more but supercritical technology carries out the water technology step, cost is than higher, thereby is difficult to obtain to use widely; Sorbent material commonly used in absorption method has gac and resin.But owing to the former expense height, the regeneration difficulty is so its use is restricted; Though latter's treatment capacity is big, also there is the problem that price is more expensive and regeneration is difficult in steady performance.Used agricultural chemicals in view of China is once long-term a large amount of, cause some stable machine chloro pesticides for a long time in the waters, soil and biological body accumulation, and constantly in environment, circulate.Therefore seek a kind of aboundresources, easy to use, it is particularly important that cheap sorbent material shows.
Summary of the invention
The object of the present invention is to provide the purposes of modified montmorillonoid, promptly as the new application of water treatment absorbent.
The modified montmorillonoid that the present invention relates to obtains by the following method:
(1) according to mass ratio 1: 49 sodium-based montmorillonite is distributed in the 490ml deionized water, stirred under the room temperature 3～4 hours, left standstill swelling 12 hours;
(2) 1.0CEC intercalator cetyl trimethylammonium bromide is dissolved in the 100ml water, makes pillaring agent;
(3) will make pillaring agent, and slowly splash in the polynite mixed solution, the dropping time was controlled at 2 hours, drip the process sodium-based montmorillonite and continue to stir suction filtration, and with deionized water wash three times with removal Br
-Plasma;
(4) 80 ℃ of oven dry are down ground, and cross 140 mesh sieves.
In fact, the present invention relates to modified montmorillonoid as the application of removing organochlorine pesticide sorbent material in the aqueous systems.
More specifically say, relate to any or multiple combination in organochlorine pesticide α-phenyl-hexachloride, organochlorine pesticide pp '-DDT, organochlorine pesticide aldrin, the organochlorine pesticide quintozene.
In order to understand essence of the present invention better, below modified montmorillonoid is further analyzed the mechanism work as sorbent material, and listed the adsorption experiment of modified montmorillonoid four kinds of organochlorine pesticides.
Polynite belongs to the inorganic nano clay, want to make it and polymkeric substance to carry out compound preparation nano composite material, at first must make organ-mmt and make the polynite surfaces externally and internally by hydrophilic change into hydrophobic, method commonly used is carried out ion-exchange with organic cation exactly makes interlamellar spacing increase simultaneously, improve the interlayer microenvironment, reduce surface energy, be beneficial between monomer or polymkeric substance insertion cheating engaging layer and form nano composite material.In general, intercalator should meet following condition:
(1) end of intercalator can form stronger chemistry or physical action with the surface of polynite, and is easy to enter the space of stratiform polynite wafer (001 face), can enlarge markedly the interlamellar spacing of polynite wafer;
(2) molecular structure of the intercalator molecule the other end should with monomer or polymer-compatible, or has a group that can react, can form stronger physics or chemical action with polymer monomer or polymer, be beneficial to the intercalation of monomer or polymkeric substance, and can improve the consistency of polymkeric substance and polynite, strengthen two alternate interface combinations, help to improve performance of composites;
(3) cheap, be easy to get, preferably existing industrial goods, intercalator commonly used have alkylammonium salt, quaternary ammonium salt, pyridine derivatives and other cationic surfactant etc.
This experiment is organic modifiers with the cetyl trimethylammonium bromide, adds a certain amount of properties-correcting agent by the calculating to loading capacity (CEC) and comes to carry out organically-modified to polynite.
1. organic modification montmonrillonite is to the Staticadsorption experiment of organochlorine pesticide α-phenyl-hexachloride
Prepare the α-Isotox solution of a series of different concns, pour in the 100ml Erlenmeyer flask that fills 0.1g soil, in 25 ℃ of water-baths, magnetic agitation, reaction 2h, centrifugal immediately 10min and suction filtration, take out the solution after 20ml filters, with the n-hexane extraction of equivalent three times, washing is separating funnel for several times.With an amount of anhydrous sodium sulfate drying, cross silica column, and with normal hexane drip washing number time, gained solution is vacuumized rotary evaporation to about 1ml under 35 ℃, shift out, wash the rotary evaporation bottle twice with a small amount of normal hexane with the 1ml transfer pipet, constant volume becomes 5ml, advances gas chromatographic detection and gets equilibrium concentration C
e, by formula: q
e=(C
0-C
E) * V/W obtains saturated adsorption capacity, q in the formula
eBe the material saturated adsorption capacity, C
0Be initial pesticide concentration, C
ePesticide concentration during for adsorption equilibrium, V are the pesticidal solutions volume, and W is the sorbing material quality.The isothermal adsorption curve is plotted in accompanying drawing 3.
2. organic modification montmonrillonite is to the Staticadsorption experiment of organochlorine pesticide pp '-DDT
Prepare the pp '-DDT pesticidal solutions of a series of different concns, pour in the 100ml Erlenmeyer flask that fills 0.1g soil, in 25 ℃ of water-baths, magnetic agitation, reaction 2h, centrifugal immediately 10min and suction filtration, take out the solution after 20ml filters, with the n-hexane extraction of equivalent three times, washing is separating funnel for several times.With an amount of anhydrous sodium sulfate drying, cross silica column, and with normal hexane drip washing number time, gained solution is vacuumized rotary evaporation to about 1ml under 35 ℃, shift out, wash the rotary evaporation bottle twice with a small amount of normal hexane with the 1ml transfer pipet, constant volume becomes 5ml, advances gas chromatographic detection and gets equilibrium concentration C
e, by formula: q
e=(C
0-C
E) * V/W obtains saturated adsorption capacity, q in the formula
eBe the material saturated adsorption capacity, C
0Be initial pesticide concentration, C
ePesticide concentration during for adsorption equilibrium, V are the pesticidal solutions volume, and W is the sorbing material quality.The isothermal adsorption curve is plotted in Fig. 4.
3. organic modification montmonrillonite is to the Staticadsorption experiment of organochlorine pesticide aldrin
Prepare the aldrin pesticidal solutions of a series of different concns, pour in the 100ml Erlenmeyer flask that fills 0.1g soil, in 25 ℃ of water-baths, magnetic agitation, reaction 2h, centrifugal immediately 10min and suction filtration take out the solution after 20ml filters, with the n-hexane extraction of equivalent three times, washing is separating funnel for several times, with an amount of anhydrous sodium sulfate drying, crosses silica column, and with normal hexane drip washing number time, gained solution is vacuumized rotary evaporation to about 1ml under 35 ℃, shift out, wash the rotary evaporation bottle twice with a small amount of normal hexane with the 1ml transfer pipet, constant volume becomes 5ml, advances gas chromatographic detection and gets equilibrium concentration C
e, by formula: q
e=(C
0-C
E) * V/W obtains saturated adsorption capacity, q in the formula
eBe the material saturated adsorption capacity, C
0Be initial pesticide concentration, C
ePesticide concentration during for adsorption equilibrium, V are the pesticidal solutions volume, and W is the sorbing material quality.The isothermal adsorption curve is plotted in Fig. 5.
4. organic modification montmonrillonite is to the Staticadsorption experiment of organochlorine pesticide quintozene
Prepare the quintozene pesticidal solutions of a series of different concns, pour in the 100ml Erlenmeyer flask that fills 0.1g soil, in 25 ℃ of water-baths, magnetic agitation, reaction 2h, centrifugal immediately 10min and suction filtration take out the solution after 20ml filters, with the n-hexane extraction of equivalent three times, washing is separating funnel for several times, with an amount of anhydrous sodium sulfate drying, crosses silica column, and with normal hexane drip washing number time, gained solution is vacuumized rotary evaporation to about 1ml under 35 ℃, shift out, wash the rotary evaporation bottle twice with a small amount of normal hexane with the 1ml transfer pipet, constant volume becomes 5ml, advances gas chromatographic detection and gets equilibrium concentration C
e, by formula: q
e=(C
0-C
E) * V/W obtains saturated adsorption capacity, q in the formula
eBe the material saturated adsorption capacity, C
0Be initial pesticide concentration, C
ePesticide concentration during for adsorption equilibrium, V are the pesticidal solutions volume, and W is the sorbing material quality.The isothermal adsorption curve is plotted in Fig. 6.
Measure by adsorption experiment four kinds of organochlorine pesticides, as sorbent material the trace organochlorine pesticide in the aqueous solution all there is extraordinary adsorption effect with organic modification montmonrillonite of the present invention, when organic chloro pesticide concentration is lower than 0.1mg/L, organo montmorillonite still has adsorption effect preferably to agricultural chemicals, and average loading capacity is 50 μ g/g.
Description of drawings
Fig. 1 is the imvite modified front and back XRD spectra that the present invention relates to, and X-coordinate is a diffraction angle, and ordinate zou is a diffraction peak intensity.
Fig. 2 is the imvite modified front and back infrared spectrogram that the present invention relates to, and X-coordinate is a wavelength, and ordinate zou is an absorption peak strength.
Fig. 1, Fig. 2 display surface promoting agent have as a result inserted between cheating engaging layer, and the orderly gathering of tensio-active agent makes interlayer form a hydrophobic region, and the existence of this hydrophobic distribution phase makes this material produce distribution absorption to the hydrophobic organic in the water.
Fig. 3 is the modified montmorillonoid that the present invention relates to isothermal adsorption curve to α-phenyl-hexachloride, and X-coordinate is an equilibrium concentration, and ordinate zou is a saturated adsorption capacity.
Fig. 4 is the modified montmorillonoid that the present invention relates to isothermal adsorption curve to pp '-DDT, and X-coordinate is an equilibrium concentration, and ordinate zou is a saturated adsorption capacity.
Fig. 5 is the modified montmorillonoid that the present invention relates to isothermal adsorption curve to aldrin, and X-coordinate is an equilibrium concentration, and ordinate zou is a saturated adsorption capacity.
Fig. 6 is the modified montmorillonoid that the present invention relates to isothermal adsorption curve to quintozene, and X-coordinate is an equilibrium concentration, and ordinate zou is a saturated adsorption capacity.
Embodiment
(1) in the 2000ml large beaker, the 10g sodium-based montmorillonite is distributed in the 490ml deionized water, stir 3～4h under the room temperature, leave standstill swelling 12h;
(2) 3.2805g (1.0CEC) cetyl trimethylammonium bromide is dissolved in the 100ml water, makes pillaring agent;
(3) pillaring agent of making is slowly splashed in the polynite mixed solution, the dropping time is controlled at 2h, drips the process sodium-based montmorillonite and continues to stir;
(4) suction filtration, and with deionized water wash three times to remove the Br-plasma;
(5) 80 ℃ of oven dry are down ground, and cross 140 mesh sieves.
Claims (2)
1. modified montmorillonoid is as the application of removing organochlorine pesticide sorbent material in the aqueous systems.
According to claim 1 modified montmorillonoid as the application of removing organochlorine pesticide sorbent material in the aqueous systems, it is characterized in that described organochlorine pesticide is any or multiple combination in organochlorine pesticide α-phenyl-hexachloride, organochlorine pesticide pp '-DDT, organochlorine pesticide aldrin, the organochlorine pesticide quintozene.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
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|---|---|---|---|
| CN 200710056729 CN101024527A (en) | 2007-02-06 | 2007-02-06 | Use of modified montmorillonite as organic chlorine farm chemicals adsorbant in dewatering system |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101219367B (en) * | 2007-09-30 | 2010-05-19 | 四川大学 | Amino acid modified montmorillonite-synthesized polymer hybridisation microsphere, preparation method and application thereof |
| CN101731493A (en) * | 2008-11-14 | 2010-06-16 | 周京石 | Production process for removing pesticide residue from extract of Ginkgo biloba |
| CN104007207A (en) * | 2014-06-18 | 2014-08-27 | 中国农业大学 | Magnetic modified nanometer organic montmorillonite and method for extracting and analyzing pesticides in water through magnetic modified nanometer organic montmorillonite |
| CN106986406A (en) * | 2017-04-17 | 2017-07-28 | 安徽建筑大学 | A kind of minimizing technology of pair of rubigan trichloroethanes |
| CN107490526A (en) * | 2017-09-06 | 2017-12-19 | 中国工程物理研究院核物理与化学研究所 | Macromolecule material aging effect the cannot-harm-detection device and its detection method |
| CN107873919A (en) * | 2017-12-25 | 2018-04-06 | 合肥市绿之林农业开发有限公司 | A kind of sunset abelmoschus flower teabag drink of low impurity |
| CN109841818A (en) * | 2019-03-05 | 2019-06-04 | 电子科技大学 | A kind of preparation method and applications of lithium secondary battery cathode material |
| CN113477227A (en) * | 2021-07-30 | 2021-10-08 | 中国环境科学研究院 | Preparation method of grafting reinforced biochar-based heavy metal adsorption material |
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2007
- 2007-02-06 CN CN 200710056729 patent/CN101024527A/en active Pending
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101219367B (en) * | 2007-09-30 | 2010-05-19 | 四川大学 | Amino acid modified montmorillonite-synthesized polymer hybridisation microsphere, preparation method and application thereof |
| CN101731493A (en) * | 2008-11-14 | 2010-06-16 | 周京石 | Production process for removing pesticide residue from extract of Ginkgo biloba |
| CN104007207A (en) * | 2014-06-18 | 2014-08-27 | 中国农业大学 | Magnetic modified nanometer organic montmorillonite and method for extracting and analyzing pesticides in water through magnetic modified nanometer organic montmorillonite |
| CN104007207B (en) * | 2014-06-18 | 2015-07-22 | 中国农业大学 | Magnetic modified nanometer organic montmorillonite and method for extracting and analyzing pesticides in water through magnetic modified nanometer organic montmorillonite |
| CN106986406A (en) * | 2017-04-17 | 2017-07-28 | 安徽建筑大学 | A kind of minimizing technology of pair of rubigan trichloroethanes |
| CN107490526A (en) * | 2017-09-06 | 2017-12-19 | 中国工程物理研究院核物理与化学研究所 | Macromolecule material aging effect the cannot-harm-detection device and its detection method |
| CN107490526B (en) * | 2017-09-06 | 2023-08-22 | 中国工程物理研究院核物理与化学研究所 | Nondestructive testing device and method for aging effect of high polymer material |
| CN107873919A (en) * | 2017-12-25 | 2018-04-06 | 合肥市绿之林农业开发有限公司 | A kind of sunset abelmoschus flower teabag drink of low impurity |
| CN109841818A (en) * | 2019-03-05 | 2019-06-04 | 电子科技大学 | A kind of preparation method and applications of lithium secondary battery cathode material |
| CN109841818B (en) * | 2019-03-05 | 2021-12-03 | 电子科技大学 | Preparation method and application of negative electrode material of lithium secondary battery |
| CN113477227A (en) * | 2021-07-30 | 2021-10-08 | 中国环境科学研究院 | Preparation method of grafting reinforced biochar-based heavy metal adsorption material |
| CN113477227B (en) * | 2021-07-30 | 2022-02-01 | 中国环境科学研究院 | Preparation method of grafting reinforced biochar-based heavy metal adsorption material |
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