CN103922435B - Aqua Folium Camelliae sinensis extract or shaddock ped water extract application and the adsorption method in Adsorption of Heavy Metal Ions - Google Patents
Aqua Folium Camelliae sinensis extract or shaddock ped water extract application and the adsorption method in Adsorption of Heavy Metal Ions Download PDFInfo
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Abstract
The invention discloses a kind of Aqua Folium Camelliae sinensis extract or shaddock ped water extract application and the adsorption method in Adsorption of Heavy Metal Ions, it is characterized in that: Aqua Folium Camelliae sinensis extract or shaddock ped water extract are added water and be mixed with water extract solution and pack in bag filter, the pH that adjusts heavy metal ion solution is acid, then bag filter is immersed in described heavy metal ion solution. The present invention utilizes natural discarded object tea dust and shaddock ped, with the heavy metal ion in Aqua Folium Camelliae sinensis extract or shaddock ped water extract absorption waste water, belongs to twice laid, with low cost; And compared with other natural adsorbents, tea dust and shaddock ped do not need special processing, and the preparation process of its water extract is simple, easy to operate; And without eco-toxicity, can not produce secondary pollution; Main, Aqua Folium Camelliae sinensis extract of the present invention or shaddock ped water extract have very superior absorption property to heavy metal ion, can application and the processing of the waste water of the field discharge such as electroplating industry, plastics industry, electronics industry, mining.
Description
Technical field
The present invention relates to Aqua Folium Camelliae sinensis extract or shaddock ped water extract application and use Aqua Folium Camelliae sinensis extract or the shaddock in Adsorption of Heavy Metal IonsThe method of severe edema due to hypofunction of the spleen extract Adsorption of Heavy Metal Ions.
Background technology
Along with the development of industrial technology, it is day by day serious that the heavy-metal pollution in industrial wastewater becomes. Its soluble-salt is along with dirtThe discharge of water and make ocean, rivers, lake and the farmland etc. of occurring in nature enjoy pollution, if do not controlled, will threatenTo the mankind's healthy and existence. Copper is the element that industrial quarters is often used, and copper ion pollutes the Important Problems that also becomes global concern.National sewage comprehensive emission standard expressly provides that the first discharge standard of copper waste water is that total copper content is less than 5.0mg/L, field irrigationWater standard is that total copper content is less than 0.5mg/L. Thereby eliminating heavy-metal pollution becomes the task of top priority.
Absorption method is to containing having demonstrated higher researching value in the wastewater treatment of heavy metal. Some are through chemical precipitations and otherThe dirty waste water containing micro heavy after treatment such as method is especially adapted to the method, makes it reach sewage drainage standard. Absorption methodThe most important thing is the selection of adsorbent. Had a lot of materials to be used to the adsorbent as heavy metal, as duck excrement (Xiang Hongzhen, oldKindly help secure the success of, Li Xiangqian, etc. the absorption-desorb research of duck excrement to Cu, Zn. Chinese agronomy circular, 2012,28 (32): 31-34),Resin cation (Zhao Shunan. resin cation is in the application of processing in effluent containing heavy metal ions. scientific and technical innovation Leader, 2012,25:144-145), (Liu Yang, waits .4A zeolite to Pb in combined pollution water body to zeolite for Jin Lanshu, Gao Xiangji2+、Cu2+And Cd2+'sRemove. environmental project journal, 2012,6 (5): 1599-1603) and other biological adsorbent (BrinzaL, DringMJ,GavrilescuM.Marinemicroandmacroalgalspeciesasbiosorbentsforheavymetals[J].EnvironmentalEngineeringandManagementJournal,2007,6(3):237-251.DasSK,DasAR,GuhaAK.AstudyontheadsorptionmechanismofmercuryonAspergillumsversicolorbiomass[J].EnvironmentalScienceandTechnology,2007,41:8281-8287.LinCC,LaiYT.AdsorptionandrecoveryofleadfromaqueoussolutionsbyimmobilizedPseudomonasaeruginosaPU21beads[J].JournalofHazardousMaterial, 2005,137 (1): 99-105) etc. But these adsorbents also exist some to ask simultaneouslyTopic, if any adsorption capacity limited, some absorption properties are not high, there is secondary pollution in what have. Therefore, for a specific huge sum of moneyBelong to, develop the society that the adsorbent high with seeking green cost performance strengthen day by day in environmental consciousness significant.
Summary of the invention
The object of the invention is, for avoiding the existing weak point of above-mentioned prior art, to utilize the water extraction of discarded natural products to getThing Adsorption of Heavy Metal Ions, provides Aqua Folium Camelliae sinensis extract and shaddock ped water extract application and the use Aqua Folium Camelliae sinensis in Adsorption of Heavy Metal IonsThe method of extract and shaddock ped water extract Adsorption of Heavy Metal Ions.
For achieving the above object, the present invention adopts following technical scheme:
Aqua Folium Camelliae sinensis extract or the application of shaddock ped water extract in Adsorption of Heavy Metal Ions, as used Aqua Folium Camelliae sinensis extract or shaddock ped water extractMake adsorbent for heavy metal, or utilize the heavy metal ion in Aqua Folium Camelliae sinensis extract or shaddock ped water extract absorption waste water, or profitBy the heavy metal ion in Aqua Folium Camelliae sinensis extract or shaddock ped water extract selective absorption solution.
Wherein, described heavy metal ion is preferably copper ion.
Described heavy metal ion exists with the form of soluble-salt, as nitrate.
The present invention uses the method for Aqua Folium Camelliae sinensis extract or shaddock ped water extract Adsorption of Heavy Metal Ions, and its feature is:
Aqua Folium Camelliae sinensis extract or shaddock ped water extract are added water and be mixed with water extract solution and pack in bag filter, adjust heavy metal ion moltenThe pH of liquid is acid, then described bag filter is immersed in described heavy metal ion solution.
The preparation method of described Aqua Folium Camelliae sinensis extract is: tea leaf powder is broken into end and adds in deionized water, extract 2～3 times at 70 DEG C,Each extraction time is 1.5～2.5 hours, and after each extraction, by centrifugal extract acquisition supernatant, merging obtains after extracting at every turnSupernatant, concentrated and freeze drying obtains Powdered Aqua Folium Camelliae sinensis extract, and sublimation drying is 16h, and condenser temperature is-40 DEG C; InstituteStating the quality of tealeaves and the volume ratio of deionized water is 1g:30ml;
The preparation method of described shaddock ped water extract is: shaddock ped is ground into end and adds in deionized water, extract 2～3 times at 80 DEG C,Each extraction time is 2.5～3.5 hours, and after each extraction, by centrifugal extract acquisition supernatant, merging obtains after extracting at every turnSupernatant, concentrated and freeze drying obtains Powdered shaddock ped water extract, and sublimation drying is 16h, and condenser temperature is-40 DEG C; InstituteStating the quality of shaddock ped and the volume ratio of deionized water is 2g:30ml;
The pH of heavy metal ion solution is adjusted into acidity, and preferably pH is 2-5. Method of adjustment is by HNO3Be mixed with concentrationFor the dilute acid soln of 0.0001-0.01mol, add in heavy metal ion solution and measure heavy metal ion solution with pH meter.
After described bag filter is immersed in heavy metal ion solution, under normal temperature, can complete absorption, variations in temperature to adsorption rate slightlyImpact, keep solution temperature be 0～50 DEG C all can, preferably 20-30 DEG C.
Utilize water extract Adsorption of Heavy Metal Ions, along with the increase of the initial concentration of heavy metal ion, the suction of Unit Weight water extractAttached capacity can increase gradually, and the concentration range of water extract solution solution of the present invention is preferably 50-200mg/L. Described heavy metalIn solion, in the mole of heavy metal ion and water extract solution, the ratio of water extract quality is 3.906～15.625mol/kg.
Water extract solution is added after heavy metal ion solution, and water extract starts Adsorption of Heavy Metal Ions at once, along with the increasing of timeAdd, adsorbance increases gradually, finally reaches balance. Control adsorption time of the present invention is 10min-1440min.
The present invention uses the method for Aqua Folium Camelliae sinensis extract or shaddock ped water extract Adsorption of Heavy Metal Ions, the detection of its adsorption rate and adsorbanceStep is as follows:
Use after water extract Adsorption of Heavy Metal Ions the outer heavy metal concentration of bag filter after heavy metal ion initial concentration solution and absorptionAdopt ICP-OES (inductively coupled plasma atomic emission) method to measure, then calculate the suction of heavy metal ion according to (1) formulaAttached rate q, according to the adsorbance X of (2) formula calculating heavy metal ion.
Wherein, the adsorption rate that q is heavy metal ion;
CoThe metal ion solution initial concentration (mg/L) of attaching most importance to, after adjusting pH, the concentration of heavy metal ion solutionAs its initial concentration;
CeFor the outer heavy metal concentration (mg/L) of bag filter after certain a period of time is carried out in absorption;
X is the adsorbance (mg/g) that heavy metal ion after certain a period of time is carried out in absorption;
CaFor water extract solution concentration (g/L);
V is the volume of water extract solution and heavy metal ion solution and (L);
VaFor water extract liquor capacity (L).
While adsorbing certain density heavy metal ion according to water extract, adsorption rate and adsorbance, with the variation of adsorption time, can be drawn outAdsorption rate and adsorbance time dependent relation curve, thus obtained equilibration time can characterize ABSORBENTS ABSORPTION metal ionAbsorption speed degree.
Compared with the prior art, beneficial effect of the present invention is embodied in:
The present invention utilizes natural discarded object tea dust and shaddock ped, with the heavy metal in Aqua Folium Camelliae sinensis extract or shaddock ped water extract absorption waste waterIon, belongs to twice laid, with low cost; And compared with other natural adsorbents, tea dust and shaddock ped do not need special locatingReason, the preparation process of its water extract is simple, easy to operate; In addition, the present invention is using Aqua Folium Camelliae sinensis extract or shaddock ped water extract as heavyThe adsorbent of metal ion, without eco-toxicity, can not produce secondary pollution; Main, Aqua Folium Camelliae sinensis extract of the present invention or shaddock pedWater extract has very superior absorption property to heavy metal ion, can application and electroplating industry, plastics industry, electronics industry,The processing of the waste water of the field discharges such as mining, has very large potential actual application value.
Brief description of the drawings
Fig. 1 is at Cu in embodiment 1-362+When the pH=2 of solution, the copper absorption rate under measured different adsorption timesCurve map;
Fig. 2 is at Cu in embodiment 1-362+When the pH=3 of solution, the copper absorption rate under measured different adsorption timesCurve map;
Fig. 3 is at Cu in embodiment 1-362+When the pH=5 of solution, the copper absorption rate under measured different adsorption timesCurve map;
Fig. 4 is the curve map of the cupric ion adsorption under the measured different adsorption times of embodiment 37-54;
Fig. 5 is the curve map of the cupric ion adsorption under the different water extract concentration of embodiment 55-90.
Detailed description of the invention
Below in conjunction with embodiment, the present invention will be further described:
Embodiment 1～36
1, prepare Aqua Folium Camelliae sinensis extract: 10g tea leaf powder is broken into end and adds in 300ml deionized water, extract 3 70 DEG C of water-bathsInferior, extract 1.5 hours at every turn, after each extraction, by centrifugal extract acquisition supernatant, merge the supernatant obtaining after each extractionLiquid, concentrated and freeze drying obtains Powdered Aqua Folium Camelliae sinensis extract, and sublimation drying is 16h, and condenser temperature is-40 DEG C;
Prepare shaddock ped water extract: 20g shaddock ped is broken into end and adds in 300ml deionized water, extract 3 times 80 DEG C of water-baths, everyInferior extraction 2.5 hours, by centrifugal extract acquisition supernatant, merges the supernatant obtaining after each extraction after each extraction, denseThe freeze drying of contracing obtains Powdered shaddock ped water extract, and sublimation drying is 16h, and condenser temperature is-40 DEG C;
2, configuration concentration is 100mgL respectively-1Aqua Folium Camelliae sinensis extract solution and shaddock ped water extract solution;
3, taking the single element mark liquid configuration concentration of Cu as 10mgL-1Cu2+Solution, and regulate pH to be respectively 2,3 and 5,And test obtains Cu after having regulated2+Initial concentration solution;
4,10ml Aqua Folium Camelliae sinensis extract solution is put into bag filter, two ends clamp with dialysis clamp, put into the Cu of 40ml2+SolutionIn (molal weight than for 6.25mol/kg), (220r/min) constant temperature (25 DEG C) vibration on reciprocation type vibrating machine, respectively at30,60,120,360,960, measure the Cu in the outer solution of bag filter when 1440min2+Concentration, averages in triplicate.
After tested, as shown in Figure 1, at the Cu of pH=22+In solution, gained adsorption rate q (AdsorptionrateofCu) complies withInferior is 4.79%, 6.16%, 7.42%, 6.94%, 6.73%, 7.15%, and maximum adsorption rate is 7.42%.
As shown in Figure 2, at the Cu of pH=32+In solution, gained adsorption rate q is followed successively by 6.45%, 8.79%, 12.08%, 12.79%,12.88%, 12.57%, maximum adsorption rate is 12.88%.
As shown in Figure 3, at the Cu of pH=52+In solution, gained adsorption rate q is followed successively by 19.69%, 34.17%, 28.11%,26.77%, 28.79%, 31.03%, maximum adsorption rate is 34.17%.
5,10ml shaddock ped water extract solution is put into bag filter, two ends clamp with dialysis clamp, put into the Cu of 40ml2+SolutionIn (molal weight than for 6.25mol/kg), (220r/min) constant temperature (25 DEG C) vibration on reciprocation type vibrating machine, respectively at30,60,120,360,960, measure the Cu in the outer solution of bag filter when 1440min2+Concentration, averages in triplicate.
After tested, as shown in Figure 1, at the Cu of pH=22+In solution, gained adsorption rate q is followed successively by 5.96%, 6.92%, 7.78%,7.93%, 8.13%, 7.86%, maximum adsorption rate is 8.13%.
As shown in Figure 2, at the Cu of pH=32+In solution, gained adsorption rate q is followed successively by 6.68%, 8.72%, 10.33%, 11.23%,10.68%, 10.72%, maximum adsorption rate is 11.23%.
As shown in Figure 3, at the Cu of pH=52+In solution, gained adsorption rate q is followed successively by 11.66%, 14.95%, 20.38%,21.95%, 24.03%, 24.41%, maximum adsorption rate is 24.41%
Embodiment 37-54
1, prepare Aqua Folium Camelliae sinensis extract: 10g tea leaf powder is broken into end and adds in 300ml deionized water, extract 2 70 DEG C of water-bathsInferior, extract 2.5 hours at every turn, after each extraction, by centrifugal extract acquisition supernatant, merge the supernatant obtaining after each extractionLiquid, concentrated and freeze drying obtains Powdered Aqua Folium Camelliae sinensis extract, and sublimation drying is 16h, and condenser temperature is-40 DEG C;
Prepare shaddock ped water extract: 20g shaddock ped is ground into end and adds in 300ml deionized water, extract 2 times 80 DEG C of water-baths,Each extraction 3.5 hours, by centrifugal extract acquisition supernatant, merges the supernatant obtaining after each extraction after each extraction,Concentrated and freeze drying obtains Powdered shaddock ped water extract, and sublimation drying is 16h, and condenser temperature is-40 DEG C;
2, configuration concentration is 100mgL respectively-1Aqua Folium Camelliae sinensis extract solution and shaddock ped water extract solution;
3, taking the single element mark liquid configuration concentration of Cu as 10mgL-1Cu2+Solution, and to regulate pH be 5;
4,10ml Aqua Folium Camelliae sinensis extract solution is put into bag filter, two ends clamp with dialysis clamp, put into the Cu of 45ml2+SolutionIn (molal weight than for 7.03mol/kg), (220r/min) constant temperature (25 DEG C) vibration on reciprocation type vibrating machine, respectively at10,30,60,100,120,240,360,720, sampling and measuring when 1440min, average in triplicate, result tableBright, the adsorbance (AdsorptionquantityofCu) of Aqua Folium Camelliae sinensis extract absorbing copper ion is respectively 49.15mg/g, 71.90mg/g,95.10mg/g，112.55mg/g，115.95mg/g，127.40mg/g，129.05mg/g，127.90mg/g，129.45mg/g。
5,10ml shaddock ped water extract solution is put into bag filter, two ends clamp with dialysis clamp, put into the Cu of 45ml2+In solution(molal weight than for 7.03mol/kg), (220r/min) constant temperature (25 DEG C) vibration on reciprocation type vibrating machine, respectively at 10,30,60,100,120,240,360,720, sampling and measuring when 1440min, average in triplicate. Result shows,The adsorbance of shaddock ped water extract absorbing copper ion is respectively 41.30mg/g, 63.70mg/g, 89.10mg/g, 99.65mg/g, 103.55Mg/g, 109.60mg/g, 113.45mg/g, 115.80mg/g, 118.05mg/g. Refer to accompanying drawing 4.
Embodiment 55-90
The present embodiment is prepared Aqua Folium Camelliae sinensis extract and shaddock ped water extract by the identical mode of embodiment 37-54;
Tealeaves and shaddock ped water extract solution concentration are 100mgL-1，Cu2+The pH of solution is 5, and concentration is 10mgL-1, get 10mLWater extract solution is put into bag filter, and two ends clamp with dialysis clamp, put into 50mlCu2+In solution, (molal weight ratio is7.8125mol/kg), (220r/min) constant temperature (25 DEG C) vibration on reciprocation type vibrating machine, the sampling and measuring time is respectively 10,30,60,100,120,240,360,720,1440min, in triplicate. Result shows, tealeaves water extraction in such casesThing is respectively 107.50mg/g to the adsorbance of copper ion, 156.55mg/g, and 145.95mg/g, 139.65mg/g, 151.50mg/g,153.22mg/g. Shaddock ped water extract is respectively 68.85mg/g to the adsorbance of copper ion, 91.80mg/g, 112.35mg/g, 119.50Mg/g, 116.34mg/g, 131.35mg/g. Other conditions are identical, change the concentration of Aqua Folium Camelliae sinensis extract and shaddock ped water extract, allFor 50mgL-1, put into 50mlCu2+In solution (molal weight is than being 15.625mol/kg), Aqua Folium Camelliae sinensis extract in such casesAdsorbance to copper ion is respectively 69.4mg/g, 89.1mg/g, 93.6mg/g, 97.5mg/g, 98.1mg/g, 97.8mg/g.Shaddock ped water extract is respectively 57.7mg/g to the adsorbance of copper ion, 80.1mg/g, and 79.8mg/g, 92.3mg/g, 88.1mg/g,91.2mg/g. Other conditions are identical, change the concentration of Aqua Folium Camelliae sinensis extract and shaddock ped water extract, are 200mgL-1, put into50mlCu2+In solution (molal weight is than being 3.906mol/kg), Aqua Folium Camelliae sinensis extract is divided the adsorbance of copper ion in such casesWei 49.25mg/g, 72.78mg/g, 103.65mg/g, 107.70mg/g, 105.93mg/g, 99.03mg/g. Shaddock ped waterExtract is respectively 32.80mg/g to the adsorbance of copper ion, 39.83mg/g, and 52.70mg/g, 62.03mg/g, 60.55mg/g,61.35mg/g. Refer to accompanying drawing 5.
Embodiment 91-92
Prepare Aqua Folium Camelliae sinensis extract and shaddock ped water extract by the identical mode of embodiment 37-54;
Get the water sample of tributary, the Fei river in Anhui Province, Hefei City section, with clearing up after Filter paper filtering, regulating its pH value is 5, gets this water sample of 40mLAs heavy metal ion solution;
Getting 10mL concentration is 100mgL-1Aqua Folium Camelliae sinensis extract solution is put into bag filter, and two ends clamp with dialysis clamp, put into waterIn sample, (220r/min) constant temperature (25 DEG C) vibration on reciprocation type vibrating machine, the sampling and measuring time is 720min, repeats threeInferior. Result shows, Aqua Folium Camelliae sinensis extract is in the time processing Fei river in Anhui Province water sample, best to the treatment effect of Cu in 6 heavy metal species ions, inhalesAttached amount maximum, is 151.50mg/g, and other 5 heavy metal species are also had to higher adsorbance. Concrete data are in table 1.
Table 1 is processed tributary, Fei river in Anhui Province water sample result by Aqua Folium Camelliae sinensis extract
Under the same terms, Aqua Folium Camelliae sinensis extract is changed into the shaddock ped water extract of same concentration, result shows, the adsorption effect of Cu and AsBest, adsorbance is respectively 116.33mg/g and 102.67. Concrete data are in table 2.
Table 2 is processed tributary, Fei river in Anhui Province water sample result with shaddock ped water extract
Embodiment 93-94
Prepare Aqua Folium Camelliae sinensis extract and shaddock ped water extract by the identical mode of embodiment 37-54;
Get Hefei City's waste water from plating plant, with clearing up after Filter paper filtering, regulating its pH value is 5, gets this water sample of 40mL;
Getting 10mL concentration is 100mgL-1Aqua Folium Camelliae sinensis extract solution is put into bag filter, and two ends clamp with dialysis clamp, put into waterIn sample, (220r/min) constant temperature (25 DEG C) vibration on reciprocation type vibrating machine, the sampling and measuring time is 720min, repeats threeInferior. Result shows, Aqua Folium Camelliae sinensis extract is in the time processing certain waste water from plating plant, and best to the absorption of Cu, adsorbance is 103.65mg/g,Other heavy metal ion are also possessed to certain adsorption capacity. Concrete data are in table 3.
Table 3 is processed certain waste water from plating plant result by Aqua Folium Camelliae sinensis extract
Under the same terms, Aqua Folium Camelliae sinensis extract is changed into the shaddock ped water extract of same concentration, result shows, shaddock ped water extract is to these six kindsThe adsorption effect of heavy metal ion is similar. Concrete data are in table 4.
Table 4 is processed certain waste water from plating plant result with shaddock ped water extract
Above-described embodiment, only for the present invention will be described, does not form the restriction to claim scope, art technology peopleOther alternative means that member can expect, all within the scope of the claims in the present invention.
Claims (4)
1. the method that uses Aqua Folium Camelliae sinensis extract or shaddock ped water extract Adsorption of Heavy Metal Ions, is characterized in that:
Aqua Folium Camelliae sinensis extract or shaddock ped water extract are added water and be mixed with water extract solution and pack in bag filter, adjust heavy metal ion moltenThe pH of liquid is 5, then described bag filter is immersed in described heavy metal ion solution.
2. the method for use Aqua Folium Camelliae sinensis extract according to claim 1 or shaddock ped water extract Adsorption of Heavy Metal Ions, its featureBe:
The preparation method of described Aqua Folium Camelliae sinensis extract is: tea leaf powder is broken into end and adds in deionized water, extract 2～3 times at 70 DEG C,Each extraction time is 1.5～2.5 hours, and after each extraction, by centrifugal extract acquisition supernatant, merging obtains after extracting at every turnSupernatant, concentrated and freeze drying obtains Powdered Aqua Folium Camelliae sinensis extract, and sublimation drying is 16h, and condenser temperature is-40 DEG C; InstituteStating the quality of tealeaves and the volume ratio of deionized water is 1g:30ml;
The preparation method of described shaddock ped water extract is: shaddock ped is ground into end and adds in deionized water, extract 2～3 times at 80 DEG C,Each extraction time is 2.5～3.5 hours, and after each extraction, by centrifugal extract acquisition supernatant, merging obtains after extracting at every turnSupernatant, concentrated and freeze drying obtains Powdered shaddock ped water extract, and sublimation drying is 16h, and condenser temperature is-40 DEG C; InstituteStating the quality of shaddock ped and the volume ratio of deionized water is 2g:30ml.
3. the method for use Aqua Folium Camelliae sinensis extract according to claim 1 or shaddock ped water extract Adsorption of Heavy Metal Ions, its featureBe: after described bag filter is immersed in heavy metal ion solution, keeping heavy metal ion solution temperature is 0～50 DEG C.
4. the method for use Aqua Folium Camelliae sinensis extract according to claim 1 or shaddock ped water extract Adsorption of Heavy Metal Ions, its featureBe: described water extract solution concentration is 50mg/L～200mg/L; The mole of heavy metal ion in described heavy metal ion solutionWith the ratio of water extract quality in water extract solution be 3.906～15.625mol/kg.
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