CN101811021A - Amphiphilic adsorbent capable of adsorbing both organic matter and heavy metal cation and preparation method thereof - Google Patents
Amphiphilic adsorbent capable of adsorbing both organic matter and heavy metal cation and preparation method thereof Download PDFInfo
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Abstract
The invention discloses an amphiphilic adsorbent capable of adsorbing both organic matter and heavy metal cations and is characterized in that the amphiphilic adsorbent is natural soil, clay mineral or zeolite modified by using an amphiphilic surfactant. The amphiphilic adsorbent has high capacity of adsorbing both organic pollutants and heavy metal cations.
Description
Technical field
The present invention relates to the amphiphilic adsorbent and the preparation thereof of a kind of while adsorb organic compound and heavy metal cation.
Background technology
Because industrial wastewater discharge, the landfill of municipal refuse discarded object is disposed, sewage is dirty irritates, multifactorial influences such as utilization of mud soil and atmospheric sedimentation, organic matter is (as benzene in the environment, phenol, aniline, multiring aromatic hydrocarbon, Deng one or more), heavy metal ion is (as cadmium, copper, zinc, plumbous, mercury, manganese, nickel, Deng one or more) combined pollution of coexistence become the principal mode of environmental pollution, these pollutants both can cause Ecological environment worsening, also may pass through Lu Sheng, hydrobiological absorption is accumulated and is entered food chain, thereby health is caused serious harm.
Absorption is the class important method that organic matter in the environment, heavy-metal pollution thing are disposed.Absorption refers in the liquid-solid or gas-solid system, and the concentrate phenomenon of the material in liquid or the gas on the surface of solids can be removed some material in gas phase or the liquid phase by absorption.The solid that is used to adsorb just is referred to as adsorbent.Adsorbent mainly be by the surface can, electrically gravitation and complexing, surface precipitation etc. one or more be used for reaching adsorbing to target substance in gas phase or the liquid phase.Said herein adsorbent refers in particular to and is used for that aqueous phase adsorbs.
The performance of adsorbent is crucial in the adsorption method, and the adsorbent with good adsorption properties can improve the ability and the efficient of removal, fixed-contamination thing from environment, has crucial effects for disposing pollutant with adsorption method.
The organic pollution in the environment and the character of heavy metal ion are opposite, organic pollution is apolar substance mostly, solubility is little and be easy to by non-polar adsorbent adsorbed in water, and heavy metal ion mainly is a polar substances, solubility is big and be easy to by polar adsorbent adsorbed in water, therefore the current adsorbent that is used for the water pollutant processing has unicity, the ABSORBENTS ABSORPTION adsorption of metal ions that just is used for adsorb organic compound is relatively poor, and the adsorbent that is used for Adsorption of Heavy Metal Ions is not suitable for yet and is adsorbed with organic pollutants.
Adopting chemical substance that the relatively poor natural adsorbent of absorption property is carried out modification is the good method that improves the natural adsorbent adsorption capacity.The employing cationic surface active agent that current application is wider carries out modification to natural clay minerals such as bentonite, vermiculites, for natural clay minerals such as improving bentonite, vermiculite organic pollutant adsorption had certain effect, but the adsorption capacity for heavy metal ion but significantly descends, studies show that for cationic heavy metal cationic dressing agent CTMAB modifies soil sample for heavy metal Cd
2+Adsorption capacity descended 40% than unmodified soil sample maximum, and reduce with the increase adsorption capacity of modifying ratio, this mainly is because organic clay mineral or the surface of modifying soil are hydrophobic surfaces, has restricted the cause of hydrophilic inorganic cation absorption.
Therefore, the shortcoming of above-mentioned cationic modified bentonitic maximum is the ability with while good adsorption organic pollution and heavy metal contaminants.
Summary of the invention
The technical problem to be solved in the present invention is that cationic organically-modified soil only has higher adsorption capacity to organic pollution and the adsorption capacity of heavy metal cation is descended.At the problems referred to above, propose to utilize amphoteric surfactant that natural soil, clay mineral and zeolite are carried out modification, prepare a class has good while adsorption capacity to organic pollution and heavy metal ion new type amphoteric adsorbent.
In order to solve the problems of the technologies described above, the invention provides the amphiphilic adsorbent of a kind of while adsorb organic compound and heavy metal cation, above-mentioned amphiphilic adsorbent is with the natural soil of amphoteric surfactant modification, clay mineral or zeolite.As preferably, above-mentioned amphoteric surfactant is the fatty alkyl dimethyl betaine, and above-mentioned natural soil pH should be in 7～9 scopes, and the surface is based on negative electrical charge, and above-mentioned clay mineral is bentonite or vermiculite.
Further, the consumption of above-mentioned amphoteric surfactant when modified natural soil, clay mineral or zeolite satisfies following formula:
M＝CEC×0.9×f×L
Wherein, the consumption of amphoteric surfactant when M is modified natural soil, clay mineral or zeolite, CEC is the cation exchange capacity of natural soil, clay mineral or zeolite, and f is that proportionality coefficient gets 0.51～0.99, and L is for desiring the quality of modified natural soil, clay mineral or zeolite.
The present invention also provides a kind of preparation method of above-mentioned amphiphilic adsorbent, it is characterized in that, comprises the steps:
1) measures the cation exchange capacity of natural soil, clay mineral or zeolite, calculate the consumption of amphoteric surfactant according to following formula: M=CEC * 0.9 * f * L
Wherein, the consumption of amphoteric surfactant when M is modified natural soil, clay mineral or zeolite, CEC is the cation exchange capacity of soil, clay mineral or zeolite, and f is that proportionality coefficient gets 0.51～0.99, and L is for desiring the quality of modified soil, clay mineral or zeolite;
2) natural soil, clay mineral or zeolite is air-dry, cross the 2mm sieve;
3) get described amount amphoteric surfactant, water-soluble, adjusting pH value is identical with the pH value of natural soil, clay mineral or zeolite, obtains the solution of amphoteric surfactant;
4) stir down, natural soil, clay mineral or zeolite are added in the solution of the described amphoteric surfactant of step 3), continue to stir, leave standstill, the supernatant that inclines obtains solid, and drying, pulverizing and cross 1～2mm sieve promptly get amphiphilic adsorbent.
The present invention also provides the another kind of preparation method of above-mentioned amphiphilic adsorbent, comprises the steps:
1) cation exchange capacity of mensuration natural soil, clay mineral or zeolite, the consumption of amphoteric surfactant when calculating modified natural soil, clay mineral or zeolite according to following formula:
M＝CEC×0.9×f×L
Wherein, M is the consumption of amphoteric surfactant, and CEC is the cation exchange capacity of soil, clay mineral or zeolite, and f is that proportionality coefficient gets 0.51～0.99, and L is for desiring the quality of modified natural soil, clay mineral or zeolite;
2) natural soil, clay mineral or zeolite is air-dry, cross the 2mm sieve;
3) get described amount amphoteric surfactant, in betaine, add entry dilution, and stir and obtain the dilution of amphoteric surfactant;
4) stir down, directly the dilution of described amphoteric surfactant is added described natural soil, clay mineral or zeolite, continue to stir in the mode of spraying, dry, pulverize and cross 1～2mm sieve, promptly get amphiphilic adsorbent.
The present invention can reach following technique effect:
With dodecyldimethylammonium hydroxide inner salt negative electrical charge soil is carried out modification, it is to heavy metal Cd
2+Energy of adsorption reach 1.3～1.8 times of unmodified soil sample, reach 4.0～8.3 times of unmodified soil sample for the energy of adsorption of organic pollution phenol.Because both sexes modification soil has and adsorbs organic, heavy metal contaminants ability simultaneously, therefore aspect environmental protection, has purposes widely.
The specific embodiment
The invention will be further described below in conjunction with specific embodiment, can be implemented so that those skilled in the art can better understand the present invention also, but illustrated embodiment is not as a limitation of the invention.
With amphoteric surfactant modified natural soil, clay mineral or zeolite, utilize and have hydrophobic group and two on the amphoteric surfactant structure simultaneously respectively with the feature of positive and negative charge hydrophilic radical, make the positive terminal of amphoteric surfactant be adsorbed on the soil surface so that soil is carried out modification, utilize the electrical gravitation of amphoteric surfactant negative electrical charge end, the N that contains lone electron pair, the coordination of O atom and five yuan or six-membered ring structure, increase is to the RETENTION BY SOILS of heavy metal ion, simultaneously the hydrophobic grouping that contains of modifier itself still keeps certain for the organic pollutant adsorption effect, thereby reaches repairing organic simultaneously, the imagination of heavy-metal composite pollution.
Prepare concrete scheme:
This programme is applicable to natural soil (pH 7～9), clay mineral or zeolite, and its surface is based on negative electrical charge, and surface modifier selects amphoteric surfactant.Main preparation flow is as follows: cation exchange capacity (cationic exchange capacity, CEC) basic data of conduct preparation of at first measuring natural soil, clay mineral or zeolite.According to the different surfactants that add different quality of soil CEC.The concrete computing formula of preparation pedotheque is as follows.
Computing formula M=CEC * 0.9 * f * L
Wherein, M is the consumption of amphoteric surfactant, CEC is the cation exchange capacity of natural soil, clay mineral or zeolite, the value of f generally gets 0.51～0.99 according to the concentration of desire absorption pollutant, proportionality coefficient f is by organic, heavy metal pollution degree value, it is high more generally to satisfy pollution level, and the principle that value is big more gets final product.In the following example for medium organic, (100～250mg/mL) press the f=0.51 value to the heavy metal pollution degree, higher organic, heavy metal pollution degree (250～400mg/mL) press the f=0.75 value, high organic, heavy metal pollution degree (＞400mg/mL) press the f=0.99 value.L is for desiring the quality of modified natural soil, clay mineral or zeolite.
Embodiment 1
With both sexes modification CEC be 280mmol/kg soil 1kg to be used to handle medium organic, heavy metal pollution degree be example, press f=0.51 and calculate.Soil should be air-dry before preparation, and cross the 2mm sieve.Take by weighing the dodecyldimethylammonium hydroxide inner salt of 129g 30% content, add in 2 premium on currency, be heated to 40～60 ℃, stirring makes the dodecyldimethylammonium hydroxide inner salt dissolving and makes solution even, adds an amount of 1mol/L HCl or 1mol/L KOH regulator solution pH value and is soil pH.Take by weighing 1kg soil, under condition of stirring, join in the dodecyldimethylammonium hydroxide inner salt solution for preparing, keep temperature to stir 2h for 40～60 ℃, stop to stir, leave standstill treat the complete sedimentation of soil after, the supernatant liquor that inclines, vacuum filtration is to doing, soil sample is transferred in the ceramic whiteware dish then, in 60～80 ℃ of oven dry, baking manually is ground into when half-dried＜bulk of 1cm, and then continues to dry by the fire to bone dry and cross 1～2mm sieve, bottling promptly obtains both sexes natural soil adsorbent.
With amphiphilic adsorbent Pyrogentisinic Acid, Cd
2+Compound sewage carries out adsorption treatment, and in the time of 30 ℃, the ratio of sewage volume and amphiphilic adsorbent quality is 10L: 1kg, and the concentration of organic pollution in the sewage (is example with phenol) is 200 μ g/ml, heavy metal is (with Cd
2+Be example) concentration be 200 μ g/ml, amphiphilic adsorbent is 48.24% to the organic pollutant adsorption rate, is 98.03% to the adsorption rate of heavy metal.
Embodiment 2
With both sexes modification CEC be 280mmol/kg soil 1kg to be used for handling high organic, heavy metal pollution degree be example, press f=0.99 calculating.Soil should be air-dry before preparation, and cross the 2mm sieve.Take by weighing the dodecyldimethylammonium hydroxide inner salt of 258g 30% content, add 100～200ml water in betaine, stirring obtains the dodecyldimethylammonium hydroxide inner salt dilution.Take by weighing 1kg soil then, under artificial or churned mechanically situation, directly be added to the dodecyldimethylammonium hydroxide inner salt dilution for preparing in the soil in the mode of spraying after, continue artificial or mechanical agitation even, stop then stirring, soil sample is transferred in the ceramic whiteware dish, in 60～80 ℃ of oven dry, baking manually is ground into when half-dried＜bulk of 1cm, and then continue to dry by the fire to bone dry, cross 1～2mm sieve, bottling promptly obtains amphiphilic adsorbent.
With amphiphilic adsorbent Pyrogentisinic Acid, Cd
2+Compound sewage carries out adsorption treatment, and in the time of 30 ℃, the ratio of sewage volume and amphiphilic adsorbent quality is 10L: 1kg, and the concentration of organic pollution in the sewage (is example with phenol) is 500 μ g/ml, heavy metal is (with Cd
2+Be example) concentration be 500 μ g/ml, amphiphilic adsorbent is 47.30% to the organic pollutant adsorption rate, is 97.75% to the adsorption rate of heavy metal.
Embodiment 3
With both sexes modification CEC be 300mmol/kg bentonite 1kg to be used to handle higher organic, heavy metal pollution degree be example, press f=0.75 and calculate.Bentonite should be air-dry before preparation, and cross the 2mm sieve.Take by weighing the dodecyldimethylammonium hydroxide inner salt of 200g 30% content, add 100～200ml water in betaine, stirring obtains the dodecyldimethylammonium hydroxide inner salt dilution.Take by weighing the 1kg bentonite then, under artificial or churned mechanically situation, directly be added to the dodecyldimethylammonium hydroxide inner salt dilution in the bentonite in the mode of spraying after, continue artificial or mechanical agitation 20min, stop then stirring, soil sample is transferred in the ceramic whiteware dish, in 60～80 ℃ of oven dry, baking manually is ground into when half-dried＜bulk of 1cm, and then continue to dry by the fire to bone dry, cross 1～2mm sieve, bottling promptly obtains the both sexes bentone adsorbent.
With amphiphilic adsorbent Pyrogentisinic Acid, Cd
2+Compound sewage carries out adsorption treatment, and in the time of 30 ℃, the ratio of sewage volume and amphiphilic adsorbent quality is 10L: 1kg, and the concentration of organic pollution in the sewage (is example with phenol) is 350 μ g/ml, heavy metal is (with Cd
2+Be example) concentration be 350 μ g/ml, amphiphilic adsorbent is 48.91% to the organic pollutant adsorption rate, is 97.51% to the adsorption rate of heavy metal.
Embodiment 4
With both sexes modification CEC be 200mmol/kg zeolite 1kg to be used to handle medium organic, heavy metal pollution degree be example, press f=0.51 and calculate.Zeolite should be air-dry before preparation, and cross the 2mm sieve.Take by weighing the dodecyldimethylammonium hydroxide inner salt of 90g 30% content, in betaine, add 100～200ml water, be heated to 40～60 ℃ and make the dodecyldimethylammonium hydroxide inner salt dissolving.Take by weighing the 1kg zeolite then, under artificial or churned mechanically situation, directly be added to the dodecyldimethylammonium hydroxide inner salt solution for preparing in the zeolite in the mode of spraying after, continue artificial or mechanical agitation 20min, stop then stirring, soil sample is transferred in the ceramic whiteware dish, in 60～80 ℃ of oven dry, baking manually is ground into when half-dried＜bulk of 1cm, and then continue to dry by the fire to bone dry, cross 1～2mm sieve, bottling promptly obtains the both sexes zeolite adsorbents.
With amphiphilic adsorbent Pyrogentisinic Acid, Cd
2+Compound sewage carries out adsorption treatment, and in the time of 30 ℃, the ratio of sewage volume and amphiphilic adsorbent quality is 10L: 1kg, and the concentration of organic pollution in the sewage (is example with phenol) is 200 μ g/ml, heavy metal is (with Cd
2+Be example) concentration be 200 μ g/ml, amphiphilic adsorbent is 32.00% to the organic pollutant adsorption rate, is 88.50% to the adsorption rate of heavy metal.
Embodiment 5
With other types both sexes modifier modification CEC be 280mmol/kg soil 1kg to be used to handle medium organic, heavy metal pollution degree be example, other both sexes modifier is example with dodecyl amino acid or lauryl imidazoline, presses f=0.51 and calculates.Soil should be air-dry before preparation, and cross the 2mm sieve.Take by weighing a certain amount of other types both sexes modifier (the dodecyl hydroxyethyl imidazole quinoline of 37g N-dodecyl alanine or 140g 40% content), add in 2 premium on currency, be heated to 60 ℃, stirring makes the dissolving of both sexes modifier and makes solution even, adds an amount of 1mol/L HCl or 1mol/L KOH regulator solution pH value and is soil pH.Take by weighing 1kg soil, under condition of stirring, join in the both sexes modifier solution for preparing, keep temperature to stir 2h for 40～60 ℃, stop to stir, leave standstill treat the complete sedimentation of soil after, the supernatant liquor that inclines, vacuum filtration is to doing, soil sample is transferred in the ceramic whiteware dish then, in 60～80 ℃ of oven dry, baking manually is ground into when half-dried＜bulk of 1cm, and then continues to dry by the fire to bone dry and cross 1～2mm sieve, bottling promptly obtains other type both sexes natural soil adsorbent.
With amphiphilic adsorbent Pyrogentisinic Acid, Cd
2+Compound sewage carries out adsorption treatment, and in the time of 30 ℃, the ratio of sewage volume and amphiphilic adsorbent quality is 10L: 1kg, and the concentration of organic pollution in the sewage (is example with phenol) is 200 μ g/ml, heavy metal is (with Cd
2+Be example) concentration be 200 μ g/ml, N-dodecyl alanine amphiphilic adsorbent is 22.22% to the organic pollutant adsorption rate, adsorption rate to heavy metal is 76.23%, dodecyl hydroxyethyl imidazole quinoline amphiphilic adsorbent is 24.15% to the organic pollutant adsorption rate, is 74.21% to the adsorption rate of heavy metal.
Comparative Examples 1
With both sexes modification CEC be 180mmol/kg soil 1kg to be used to handle medium organic, heavy metal pollution degree be example, press f=0.10 and calculate.Soil should be air-dry before preparation, and cross the 2mm sieve.Take by weighing the dodecyldimethylammonium hydroxide inner salt of 16.2g 30% content, add in 2 premium on currency, be heated to 40～60 ℃, stirring makes the dodecyldimethylammonium hydroxide inner salt dissolving and makes solution even, adds an amount of 1mol/L HCl or 1mol/L KOH regulator solution pH value and is soil pH.Take by weighing 1kg soil, under condition of stirring, join in the dodecyldimethylammonium hydroxide inner salt solution for preparing, keep temperature to stir 2h for 40～60 ℃, stop to stir, leave standstill treat the complete sedimentation of soil after, the supernatant liquor that inclines, vacuum filtration is to doing, soil sample is transferred in the ceramic whiteware dish then, in 60～80 ℃ of oven dry, baking manually is ground into when half-dried＜bulk of 1cm, and then continues to dry by the fire to bone dry and cross 1～2mm sieve, bottling promptly obtains amphiphilic adsorbent.
With amphiphilic adsorbent Pyrogentisinic Acid, Cd
2+Compound sewage carries out adsorption treatment, and in the time of 30 ℃, the ratio of sewage volume and amphiphilic adsorbent quality is 10L: 1kg, and the concentration of organic pollution in the sewage (is example with phenol) is 200 μ g/ml, heavy metal is (with Cd
2+Be example) concentration be 200 μ g/ml, amphiphilic adsorbent is 12.50% to the organic pollutant adsorption rate, is 75.50% to the adsorption rate of heavy metal.
Comparative Examples 2
Natural soil (CEC=200mmol/kg) 1kg dry, that cross 100 mesh sieves is poured in the cationic surfactant ctmab solution that 2500mL contains 72g, at 60 ℃ of stirred in water bath 2h, product after filtration, with quantitative distilled water washing 2 times, after filter is done,, about 110 ℃, activate 1h again 80～90 ℃ of oven dry down, grind the back and cross 100 mesh sieves, make cationic adsorption agent.
With cationic natural soil adsorbent Pyrogentisinic Acid, Cd
2+Compound sewage carries out adsorption treatment, and in the time of 30 ℃, the ratio of sewage volume and amphiphilic adsorbent quality is 10L: 1kg, and the concentration of organic pollution in the sewage (is example with phenol) is 500 μ g/ml, heavy metal is (with Cd
2+Be example) concentration be 500 μ g/ml, amphiphilic adsorbent is 59.02% to the organic pollutant adsorption rate, is 58.48% to the adsorption rate of heavy metal.
With empgen BB negative electrical charge soil is carried out modification, it is to heavy metal Cd
2+Energy of adsorption reach 1.3～1.8 times of unmodified soil sample, reach 4.0～8.3 times of unmodified soil sample for the energy of adsorption of organic pollution phenol.Because both sexes modification soil has and adsorbs organic, heavy metal contaminants ability simultaneously, therefore aspect environmental protection, has purposes widely.As, (1) can be used as the processing that a kind of high-efficiency adsorbent is used for heavy metal, organic compound contaminated waste water, removes heavy metal, organic matter harmful substance in the water; (2) be used to prevent the impervious barrier material of the downward seepage of liquid as refuse landfill or other places, prevent the downward seepage of heavy metal, organic matter in the liquid; (3) as the inhibitor of organic matter, heavy-metal composite pollution in farmland or the forest land, organic matter, heavy metal shift by plant absorbing or to underground water in the control soil; Or the like.
The above embodiment is the preferred embodiment that proves absolutely that the present invention lifts, and protection scope of the present invention is not limited thereto.Being equal to that those skilled in the art are done on basis of the present invention substitutes or conversion, all within protection scope of the present invention.Protection scope of the present invention is as the criterion with claims.
Claims (7)
1. the amphiphilic adsorbent of adsorb organic compound and heavy metal cation simultaneously is characterized in that described amphiphilic adsorbent is with the natural soil of amphoteric surfactant modification, clay mineral or zeolite.
2. amphiphilic adsorbent according to claim 1 is characterized in that, the consumption of described amphoteric surfactant when modified natural soil, clay mineral or zeolite satisfies following formula:
M＝CEC×0.9×f×L
Wherein, the consumption of amphoteric surfactant when M is modified natural soil, clay mineral or zeolite, CEC is the cation exchange capacity of natural soil, clay mineral or zeolite, and f is that proportionality coefficient gets 0.51～0.99, and L is for desiring the quality of modified natural soil, clay mineral or zeolite.
3. amphiphilic adsorbent according to claim 1 is characterized in that, described amphoteric surfactant is the fatty alkyl dimethyl betaine, and the carbon chain lengths of described alkyl is between eight to 18.
4. amphiphilic adsorbent according to claim 1 is characterized in that, described natural soil pH should be in 7～9 scopes, and the surface is based on negative electrical charge.
5. amphiphilic adsorbent according to claim 1 is characterized in that, described clay mineral is bentonite, vermiculite.
6. the preparation method of the described amphiphilic adsorbent of claim 1 is characterized in that, comprises the steps:
1) cation exchange capacity of mensuration natural soil, clay mineral or zeolite, the consumption of amphoteric surfactant when calculating modified natural soil, clay mineral or zeolite according to following formula:
M＝CEC×0.9×f×L
Wherein, M is the consumption of amphoteric surfactant, and CEC is the cation exchange capacity of natural soil, clay mineral or zeolite, and f is that proportionality coefficient gets 0.51～0.99, and L is for desiring the quality of modified natural soil, clay mineral or zeolite;
2) natural soil, clay mineral or zeolite is air-dry, cross the 2mm sieve;
3) get described amount amphoteric surfactant, water-soluble, the adjusting pH value of water solution is identical with the pH value of natural soil, clay mineral or zeolite, obtains the solution of amphoteric surfactant;
4) stir down, natural soil, clay mineral or zeolite are added in the solution of the described amphoteric surfactant of step 3), continue to stir, leave standstill, the supernatant that inclines obtains solid, and drying, pulverizing and cross 1～2mm sieve promptly get amphiphilic adsorbent.
7. the preparation method of the described amphiphilic adsorbent of claim 1 is characterized in that, comprises the steps:
1) cation exchange capacity of mensuration natural soil, clay mineral or zeolite, the consumption of amphoteric surfactant when calculating modified natural soil, clay mineral or zeolite according to following formula:
M＝CEC×0.9×f×L
Wherein, M is the consumption of amphoteric surfactant, and CEC is the cation exchange capacity of soil, clay mineral or zeolite, and f is that proportionality coefficient gets 0.51～0.99, and L is for desiring the quality of modified natural soil, clay mineral or zeolite;
2) natural soil, clay mineral or zeolite is air-dry, cross the 2mm sieve;
3) get described amount amphoteric surfactant, add the entry dilution, and stir, obtain the dilution of amphoteric surfactant;
4) stir down, directly the dilution of described amphoteric surfactant is added in described natural soil, clay mineral or the zeolite, continue to stir in the mode of spraying, dry, pulverize and cross 1～2mm sieve, promptly get amphiphilic adsorbent.
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