CN102874888A - Method for fixing heavy metal ions via microwave irradiation activated carbon by using humic acid as additive - Google Patents
Method for fixing heavy metal ions via microwave irradiation activated carbon by using humic acid as additive Download PDFInfo
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- CN102874888A CN102874888A CN2011101948031A CN201110194803A CN102874888A CN 102874888 A CN102874888 A CN 102874888A CN 2011101948031 A CN2011101948031 A CN 2011101948031A CN 201110194803 A CN201110194803 A CN 201110194803A CN 102874888 A CN102874888 A CN 102874888A
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- heavy metal
- gac
- humic acid
- metal ion
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Abstract
The invention discloses a method for fixing heavy metal ions via microwave irradiation activated carbon by using humic acid as an additive. The method comprises the steps of adsorbing the heavy metal ions and the humic acid on the activated carbon simultaneously; irradiating the activated carbon absorbed the heavy metal ions and the humic acid with the microwave, wherein the activated carbon used as a microwave absorbing material heats up rapidly under the action of the microwave irradiation; and reducing the heavy metal ions through carbon reducing action and fixing the heavy metal ions to the activated carbon and a humic acid structure. The activated carbon treated by the microwave can be repeatedly used. In the embodiments, the activated carbon used for fixing the Cu2+ ions can be ultimately disposed by a safe landfill way after being used. The method can also be used for treating waste water containing the heavy metal ions such as Cd2+, Cr6+, Zn2+, Pb2+, etc. The method is short in treating time, has good fixing effect, and can realize rapid treatment for industrial waste water containing the heavy metal ions.
Description
Technical field
The present invention relates to heavy metal contamination control techniques field, relate in particular to the fixedly method of heavy metal of a kind of microwave exposure gac take humic acid as additive.
Background technology
Heavy metal contamination extensively is present in the trade effluent, and the waste water of each technical process discharging of printing and dyeing, process hides, metallurgy etc. all contains the heavy metal ion of high density.Be not discharged in the environment if these waste water are treated, will the severe contamination river, lake, soil and groundwater.Heavy metal ion by tap water and in fish, shellfish and plant materials the approach such as enrichment enter human body, can cause irreversible damage to human organ, have a strong impact on human health.Comprise absorption, coagulation and ion-exchange etc. for the processing of heavy metals in industrial wastewater ion method commonly used at present, but there are secondary pollution problems in sorbent material, coagulating agent and ion exchange resin etc. after using, therefore be badly in need of exploring corresponding technology sorbent material, coagulating agent and ion exchange resin etc. after using are processed, thoroughly solve the heavy metal pollution problem that trade effluent brings.
In recent years, microwave radiation has caused chemist's extensive concern because the heating efficiency of its molecular level can cause all even fast thermal responses.Microwave is widely used in family, industry and pharmaceutical industries, in fields such as organic synthesis, product dehydrate, inorganic materials preparation, biotechnology exploitation, Analysis of environmental samples and food sterilizings, all relevant for the report of microwave application.Microwave also has report in the application of polluting control field, processes the reparation that is used to polycyclic aromatic hydrocarbon pollution such as microwave exposure, also is used to contain mud and the packing treatment of wastes produced of heavy metal.Because gac is a kind of extraordinary microwave absorbing material, its temperature can raise rapidly under microwave action, and at high temperature carbon material itself has good reductive action, the scholar is arranged recently with microwave and the activated carbon combined processing that is applied to organic pollutants, but more rare for the treatment of heavy metal ion in the water is in particular for fixedly yet there are no report to heavy metal ion.
Summary of the invention
The purpose of this invention is to provide short, good fixing effect of a kind for the treatment of time with humic acid as the fixing method of heavy metal ion of the microwave exposure gac of additive.
The technical solution adopted in the present invention is as follows:
Of the present invention with humic acid as the fixing method of heavy metal ion of the microwave exposure gac of additive, humic acid and the heavy metal ion of using first in the charcoal absorption water, then will adsorb saturated gac drying and be placed in the microwave reactor, carry out irradiation with microwave.Microwave exposure process gac is warming up to rapidly comparatively high temps, can realize simultaneously to the regeneration of gac with to the reduction of heavy metal ion, fixing.Humic acid promotes gac counterweight metal biosorption on the one hand, has also promoted on the other hand the fixed action of microwave exposure to heavy metal ion on the gac.Gac after the microwave treatment is used for the absorption to water heavy metal ion and humic acid repeatedly.Gac repeatedly uses and can carry out ultimate disposal by the mode of security landfill or high temperature incineration after microwave treatment.
The beneficial effect that the present invention has is:
1. the present invention has good fixed effect to the heavy metal ion of adsorbing on the gac, obviously reduces it as the biological effectiveness of heavy metal after the solid waste discharging, thereby reduces or eliminate its potential bio-toxicity.
2. it is aobvious that the present invention utilizes the spy that gac heats up rapidly under the microwave exposure, effectively reduces treatment time and energy consumption.
3. microwave exposure has good regeneration to gac, and the gac after the regeneration can repeated multiple timesly use, and is used further to Adsorption of Heavy Metal Ions or other pollutents.
Embodiment
Of the present invention with humic acid as the fixing method of heavy metal ion of the microwave exposure gac of additive, its better embodiment is, comprise adsorption process and heavy metal ion fixation procedure, in heavy metal ion fixation procedure process, after adsorbing saturated gac oven dry, carry out microwave exposure.
The microwave exposure treating processes mainly is that the heavy metal ion of adsorbing on the gac is reduced fixing and gac is regenerated.After microwave treatment, adopt the toxotest program (TCLP) of standard to estimate microwave exposure to the fixed action of heavy metal ion, utilize the method evaluation microwave exposures such as adsorption isothermal line, iodine sorption value and specific surface area analysis instrument to the regeneration of gac.
Usually the ature of coal cylindrical particle gac diameter that adopts among the present invention is about 0.5～3.0mm, and length is between 1～10mm; Humic acid concentration is 0～20mg/L in the original solution, and concentration of heavy metal ion is generally less than 100mg/L; Microwave uses as required flexible of power, microwave irradiation time 0～60min.
Employed gac can be granulated active carbon among the present invention, also can be powder art gac; The gac material can be ature of coal, also can be that other materials is made, such as shell, timber etc.
The handled heavy metal ion of the present invention can be Cu
2+, Cd
2+, Pb
2+, Cr
6+, Zn
2+In one or more.
Among the present invention, microwave resonator can be one-mode cavity or multimode cavity; The power range of microwave generator is regulated according to the amount of processing gac from several hectowatts to tens kilowatt;
Selected microwave frequency is 2450MHz or 915MHz etc., and mini-reactor can be used 2450MHz, and large-scale reactor can be used 915MHz;
Reactor can be made by the material that silica glass, pottery, tetrafluoroethylene, polystyrene etc. can see through microwave and can tolerate certain temperature, accept equal microwave radiation equal angles consideration everywhere from processing and easy to operate, reactor, determine the round shape that is shaped as of reactor;
Periphery at reactor and microwave generator arranges shielding case, and connects ground wire, prevents that micro-wave energy from leaking;
The mensuration of the interior temperature of charge of reactor can adopt armouring K-type thermopair and electronic temp indicator in the microwave processing process, also can adopt fibre optic temperature sensor or infrared thermometer.
The above; only for the better embodiment of the present invention, but protection scope of the present invention is not limited to this, anyly is familiar with those skilled in the art in the technical scope that the present invention discloses; the variation that can expect easily or replacement all should be encompassed within protection scope of the present invention.
Specific embodiment:
Cu in the microwave exposure gac fixed-analog waste water take humic acid as additive
2+:
With cupric chloride crystal configuration Cu
2+Storing solution; With the pure humic acid solid of the NaOH solution soluble chemistry of 0.1M, obtain the humic acid storing solution behind the membrane filtration with 0.45 μ m.
Concrete steps are as follows:
The first step: absorption.Erlenmeyer flask dose volume with 250mL is 100mL, Cu
2+Be respectively the mixing solutions of 97.6mg/L and 8.73mg/L with humic acid concentration, add 10g ature of coal columnar activated carbon, at 25 ℃, the shaking table of the 100rpm 24h that vibrates, filter.99.9% Cu in the solution after testing
2+Be adsorbed onto on the gac.
Second step: charging.Select the cylindrical reactor of silica glass material, internal diameter 4cm, height 37cm is with above-mentioned humic acid and the Cu of having adsorbed
2+And through the gac of the 105 ℃ of oven dry reactor of packing into.
The 3rd step: start microwave reactor.The microwave power of selecting is 750W, irradiation time 10min, it is suitable for reading to seal reactor with aluminium-foil paper in the reaction process, prevent pressure excessive cause the blast, the steam that produces in the treating processes is by condenser system, fluid collection vials, and through alkali lye (0.1N NaOH) and acetone mixed solvent (1: 1, it was emptying afterwards v/v) divide two-stage to absorb.
The 4th step: fixed effect detects.Adopt toxicity to leach program (TCLP) to the gac behind the microwave exposure and estimate, atomic absorption spectrophotometer records the Cu in the leach liquor
2+Concentration is 0.9mg/L, and calculating fixed percentage is 97.5%.
The 5th step: adopt new gac to repeat three circulations of the above-mentioned the first step to the three steps operation, still can be with the Cu of solution 99.7% when the gac behind the discovery micro wave regeneration is used for absorption for the third time
2+Be adsorbed onto on the charcoal; Then utilized for the 4th step to the check of the gac behind the Reusability three times fixed effect, record Cu in the leach liquor
2+Concentration be 30.9mg/L, still be lower than the Cu of solid waste security landfill
2+Leaching standard (50mg/L).
Among the present invention, because microwave is interior heating, micro-wave energy directly acts on the gac as fixing agent, and short and good fixing effect for the treatment of time reduces secondary pollution; Gac after the microwave treatment can reuse, and reduces processing cost; Microwave frequency and irradiation time, gac material, reactor material etc. have multiple choices, are convenient to select suitable reaction parameter for different heavy metal ion; Control is convenient in microwave heating, starts the microwave immediate response, closes microwave reaction and stops at once, without lag-effect.
Claims (8)
1. the fixing method of heavy metal ion of the microwave exposure gac take humic acid as additive, comprise the processing of charcoal absorption and microwave exposure, it is characterized in that, use first the heavy metal ion in the charcoal absorption water, adsorb saturated gac and utilize microwave exposure to process.
2. the fixing method of heavy metal ion of the microwave exposure gac take humic acid as additive according to claim 1, it is characterized in that, add humic acid in the charcoal absorption forward direction aqueous solution, promote gac counterweight metal biosorption effect and follow-up microwave exposure to the fixed action of the heavy metal ion of adsorbing on the gac.
3. the fixing method of heavy metal ion of the microwave exposure gac take humic acid as additive according to claim 2; it is characterized in that; described gac comprises Powdered Activated Carbon and granulated active carbon, and the material of gac comprises the various materials such as ature of coal, timber, shell.
4. according to claim 1, the fixing method of heavy metal ion of 2 or 3 described microwave exposure gacs take humic acid as additive, it is characterized in that, comprise step:
In the pending waste water that contains various heavy metal ion, add a certain amount of humic acid, by the heavy metal ion in the static or dynamic mode usefulness charcoal absorption water, utilize the mode of microwave exposure to process after adsorbing saturated gac drying, gac after the microwave treatment is recycled and reused for the absorption to heavy metal ion in the water, to repeatedly using and carrying out heavily can belonging to leaching test through the gac employing standard program of microwave treatment, for the security landfill of carrying out that meets the security landfill requirement, do not carry out ultimate disposal as Hazardous wastes in the mode of burning for what meet the security landfill requirement.
5. the fixing method of heavy metal ion of the microwave exposure gac take humic acid as additive according to claim 4 is characterized in that described microwave frequency is 2450MHz or 915MHz.
6. the fixing method of heavy metal ion of the microwave exposure gac take humic acid as additive according to claim 4, it is characterized in that, absorption saturated activity charcoal is carried out microwave exposure process the material that used reactor can see through microwave by silica glass, pottery, tetrafluoroethylene etc. and can tolerate certain temperature and make.
7. the fixing method of heavy metal ion of the microwave exposure gac take humic acid as additive according to claim 4 is characterized in that, handled heavy metal ion comprise following one or more:
Cu
2+、Cd
2+、Pb
2+、Cr
6+、Zn
2+
8. the fixing method of heavy metal ion of the microwave exposure gac take humic acid as additive according to claim 4 is characterized in that described pre-treatment step comprises:
Remove suspended substance by modes such as precipitation, air supporting or filtrations.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2011101948031A CN102874888A (en) | 2011-07-13 | 2011-07-13 | Method for fixing heavy metal ions via microwave irradiation activated carbon by using humic acid as additive |
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|---|---|---|---|
| CN2011101948031A CN102874888A (en) | 2011-07-13 | 2011-07-13 | Method for fixing heavy metal ions via microwave irradiation activated carbon by using humic acid as additive |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106396957A (en) * | 2016-09-07 | 2017-02-15 | 无限极（中国）有限公司 | Additive for planting shiitake mushrooms and shiitake mushroom planting method |
| CN106732434A (en) * | 2017-01-24 | 2017-05-31 | 福州大学 | A kind of method that acticarbon is prepared based on humic acid dipping |
| CN108452776A (en) * | 2018-04-13 | 2018-08-28 | 沈阳建筑大学 | A kind of adsorbent for sewage disposal |
| CN109364883A (en) * | 2018-10-31 | 2019-02-22 | 北京师范大学 | A kind of humic acid modified Nano Fe2O3Material preparation method and the application for removing estradiol |
| CN109535752A (en) * | 2018-11-12 | 2019-03-29 | 陕西科技大学 | A kind of carbon wafer array light absorbent and preparation method thereof |
| CN112827475A (en) * | 2020-12-30 | 2021-05-25 | 东北农业大学 | Preparation method and application of artificial humic acid functionalized colloid-like magnetic biochar |
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| US6187988B1 (en) * | 1999-02-26 | 2001-02-13 | Chang Yul Cha | Process for microwave decomposition of hazardous matter |
| CN1562775A (en) * | 2004-04-15 | 2005-01-12 | 大连理工大学 | Restoring method of activated carbon for decomposing, processing and adsorbing organic substance in waste water through microwave irradiation |
| TW200619152A (en) * | 2004-12-09 | 2006-06-16 | zhong-xin Wu | Method for recovering the heavy metals in the sludge by microwave |
-
2011
- 2011-07-13 CN CN2011101948031A patent/CN102874888A/en active Pending
Patent Citations (3)
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|---|---|---|---|---|
| US6187988B1 (en) * | 1999-02-26 | 2001-02-13 | Chang Yul Cha | Process for microwave decomposition of hazardous matter |
| CN1562775A (en) * | 2004-04-15 | 2005-01-12 | 大连理工大学 | Restoring method of activated carbon for decomposing, processing and adsorbing organic substance in waste water through microwave irradiation |
| TW200619152A (en) * | 2004-12-09 | 2006-06-16 | zhong-xin Wu | Method for recovering the heavy metals in the sludge by microwave |
Non-Patent Citations (2)
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|---|
| T. TERDKIATBURANA等: "Competition and complexation of heavy metal ions and humic acid on zeolitic MCM-22 and activated carbon", 《CHEMICAL ENGINEERING JOURNAL》 * |
| 郑文娟 等: "微波辐射回用活性炭对水中亚甲基蓝和Cd2+去除效果的研究", 《环境工程学报》 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106396957A (en) * | 2016-09-07 | 2017-02-15 | 无限极（中国）有限公司 | Additive for planting shiitake mushrooms and shiitake mushroom planting method |
| CN106732434A (en) * | 2017-01-24 | 2017-05-31 | 福州大学 | A kind of method that acticarbon is prepared based on humic acid dipping |
| CN108452776A (en) * | 2018-04-13 | 2018-08-28 | 沈阳建筑大学 | A kind of adsorbent for sewage disposal |
| CN109364883A (en) * | 2018-10-31 | 2019-02-22 | 北京师范大学 | A kind of humic acid modified Nano Fe2O3Material preparation method and the application for removing estradiol |
| CN109535752A (en) * | 2018-11-12 | 2019-03-29 | 陕西科技大学 | A kind of carbon wafer array light absorbent and preparation method thereof |
| CN109535752B (en) * | 2018-11-12 | 2020-10-27 | 陕西科技大学 | Carbon sheet array light absorption material and preparation method thereof |
| CN112827475A (en) * | 2020-12-30 | 2021-05-25 | 东北农业大学 | Preparation method and application of artificial humic acid functionalized colloid-like magnetic biochar |
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Application publication date: 20130116 |