CN102527087A - Method for absorbing and recycling heavy metals by using persimmon tannins - Google Patents
Method for absorbing and recycling heavy metals by using persimmon tannins Download PDFInfo
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- CN102527087A CN102527087A CN2012100436702A CN201210043670A CN102527087A CN 102527087 A CN102527087 A CN 102527087A CN 2012100436702 A CN2012100436702 A CN 2012100436702A CN 201210043670 A CN201210043670 A CN 201210043670A CN 102527087 A CN102527087 A CN 102527087A
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- collagen fibers
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Abstract
The invention discloses a method for absorbing and recycling heavy metals by using persimmon tannins. The absorbing material used in the method is prepared by the steps of: firstly dissolving cowhide collagen fibers and persimmon powder in water, reacting, adding glutaraldehyde or formaldehyde, reacting at the temperature of 50 DEG C and filtering, drying in vacuum and grinding. According to the method for absorbing and recycling the heavy metal, a chromatographic analytical column adsorption method is adopted to absorb and recycle precious metal, such as copper, iron, chrome and silver, wherein the average adsorption rate is above 95%. The method is applied to the absorbing and recycling treatments of a plurality of heavy metal ions in industrial wastewater with low concentration (less than 1000mg/L); and the method is low in the operating cost, can be reused and has no secondary pollution to the environment.
Description
Technical field
The absorption that the present invention relates to heavy metal is reclaimed, and the method for heavy metal is reclaimed in particularly a kind of persimmon tannin sorbing material absorption.
Background technology
At present, handle the method that contains precious metal waste water, waste residue both at home and abroad and mainly contain three kinds: the one, chemical precipitation method, the 2nd, biological treatment, the 3rd, absorption method.
Chemical precipitation method is because the deposit of heavy metal ion that precipitation reaction produces, and landfill is normally carried out in final disposal, thereby toxic heavy metal is to the pollution of environment long-term existence still, and essence is a kind of transfer of pollution in fact.The present many places of biological treatment are in the experimental study stage, and majority rests in the discussion of influence factor, also have sizable distance from industrial applications.Absorption method is to handle the particularly comparatively effective method of low-concentration heavy metal ion waste water of effluent containing heavy metal ions.Sorbing material commonly used comprises active carbon, synthetic resin, mineral matter, microorganism and natural biomass etc.; The Zhang Huiping of South China Science & Engineering University, people's results of study such as Zhu Liguo show: activated carbon fiber is to Cu
2+, Ni
2+Saturated extent of adsorption be respectively 5.1mg/g, 6.6mg/g, the activated carbon fiber of modification is to Cu
2+, Ni
2+Saturated extent of adsorption reach 20.6mg/g, 8.0mg/g, adsorption capacity is still less than normal; This method also comes with some shortcomings in industrial applications: the one, and adsorption capacity is lower, only has suction-operated and adsorption capacity less to a few metal ion like active carbon, usually between 5-20mg/g.The 2nd, absorption and desorption rate are slow, and present employed sorbing material mainly depends on the porous character of sorbing material itself, and heavy metal ion mainly is adsorbed through the surface that gets into the sorbing material endoporus, so its adsorption rate is slower.The 3rd, can't regenerate and reuse after a lot of sorbing material absorption are saturated, can only carry out processing such as landfill or burning as solid waste, often cause secondary pollution.
Summary of the invention
Technical problem to be solved by this invention provides a kind of precious metal sorbing material and adsorption recovery method with high-adsorption-capacity and good stability; A plurality of ortho positions phenolic hydroxyl group that this method utilizes tannin to have; It can be combined and complexing with multiple metal ion generation static; Willing characteristic adopts the tannin in the puckery persimmon powder to combine formation to solidify the persimmon tannin sorbing material with the animal skin glue fibrillation through aldehyde is crosslinked; And can be through modification, under various conditions, can the selective absorption precious metal ion, adsorption capacity is big, and easy desorption and be used for separating, reclaiming noble metal, and can be recycled.
The technical scheme that realizes the object of the invention is:
A kind of method of utilizing the absorption of persimmon tannin sorbing material to reclaim heavy metal comprises the steps:
(1) certain heavy metal solution of 5 groups of variable concentrations of configuration is made its calibration curve with spectrophotometer, and is obtained its concentration-absorbance fit equation, degree of fitting R through linear fit
2Greater than 0.999;
The cattle-hide collagen fibers of (2) getting certain mass is solidified the persimmon tannin sorbing material; Soaked 24 hours with deionized water, place the heavy metal solution of step (1) initial concentration then, the pH value of regulator solution is 6.0; Adopt sonic oscillation; The chromatographic analysis post of packing into then adopts the mode of dress column packing, Static Adsorption;
(3) with spectrophotometric instrumentation process adsorbed solution absorbance; Through certain heavy metal calibration curve and the concentration-absorbance fit equation of having made; The concentration after certain heavy metal solution is adsorbed can be obtained, the adsorption rate of cattle-hide collagen fibers curing persimmon tannin sorbing material can be got heavy metal through calculating;
(4) adopt strong acid solution or the EDTA of 0.01mol/L to carry out desorb, when will the adsorbent after desorb adsorbing heavy metal once more, its absorption property is constant basically.
Described cattle-hide collagen fibers solidified tannin adsorptive material, adopt the following steps preparation:
(1) takes by weighing 2 ~ 5 parts of the cattle-hide collagen fibers handled and 5 ~ 8 parts of persimmon powders, join mixed dissolution in the distilled water, stirred at normal temperatures 10 ~ 20 hours;
(2) add 3 ~ 8 parts of crosslinking agents, the pH of mixed solution is adjusted to 6.0 ~ 6.6, reacted at normal temperatures 1 ~ 3 hour with NaOH or the HCl aqueous solution; Crosslinking agent can be glutaraldehyde or formaldehyde;
(3) reacted product is put in the there-necked flask, 50 ~ 60 ℃ of following water-baths 3 ~ 5 hours;
(4) take out filtration, 60 ℃ of following vacuum drying; Taking-up is ground into fine powder with pulverizer, obtains cattle-hide collagen fibers and solidifies the persimmon tannin sorbing material.
Said cattle-hide collagen fibers and persimmon powder are prior art.
Advantage of the present invention is:
1 physical stability is good: the thermal denaturation temperature that records the curing persimmon tannin sorbing material that several groups of different persimmon powders and cattle-hide collagen fibers proportioning make with the DSC differential scanning calorimetry is respectively 156.9 ~ 175.2 ℃, 160.7 ~ 177.7 ℃, 148.1 ~ 179.1 ℃; It is much higher to compare the thermal denaturation temperature that has the research of reporting to solidify hair Baybery tannin (90～96 ℃) or curing larch tannin (93～98 ℃), promptly has higher heat endurance;
2 adsorption rates are high; Adsorption capacity is big: with active carbon, sorbing materials such as mineral matter can only adsorb a few metal ion and absorption is slow, are difficult for desorb; Adsorption capacity is less to be compared; The scope of application of solidifying the persimmon tannin adsorbent wants big, multiple metal ion has all been demonstrated the good adsorption performance, like heavy metals such as copper, iron, chromium, cadmiums.Average adsorption rate has reached more than 95%;
3 costs are low: this method adopts persimmon powder to compare tradition with the sorbing material that materials with hide glue fibril is produced and makes many that costs such as spent ion exchange resin or synthetic resin will be low;
4 is environment friendly and pollution-free: carry out landfill or burning after making heavy metal ion generate water-fast deposit with chemical precipitation method in the industry; Essence but is a kind of transfer of pollution; By contrast; The raw material of this method are natural persimmon powder and collagenous fibres, are easier to desorption after absorption is used and can produce secondary pollution to environment;
5 can be recycled: this method all can recycle multiple precious metal ion; After different stripping liquid desorbs; Sample to obtaining adsorbs again, three absorption property tests, and the result shows; Adsorbance descends to some extent but is also not obvious, explains that this product has good regenerability.
The specific embodiment
Cattle-hide collagen fibers solidified tannin adsorptive material described in the following embodiment, adopt the method that comprises the steps to process:
(1) takes by weighing 2 ~ 5 parts of the cattle-hide collagen fibers handled and 5 ~ 8 parts of persimmon powders, join mixed dissolution in the distilled water, stirred at normal temperatures 10 ~ 20 hours;
(2) add 3 ~ 8 parts of crosslinking agents, the pH of mixed solution is adjusted to 6.0 ~ 6.6, reacted at normal temperatures 1 ~ 3 hour with NaOH or the HCl aqueous solution; Crosslinking agent can be glutaraldehyde or formaldehyde;
(3) reacted product is put in the there-necked flask, 50 ~ 60 ℃ of following water-baths 3 ~ 5 hours;
(4) take out filtration, 60 ℃ of following vacuum drying; Taking-up is ground into fine powder with pulverizer, obtains cattle-hide collagen fibers and solidifies the persimmon tannin sorbing material.
Embodiment 1:
The cattle-hide collagen fibers for preparing is solidified the persimmon tannin sorbing material be used for absorbing copper, operating procedure is following:
1, the CuSO of 5 groups of variable concentrations of configuration
4Solution is made Cu with spectrophotometer
2+Calibration curve, and obtain its concentration-absorbance fit equation, degree of fitting R through linear fit
2Greater than 0.999;
2, get the prepared persimmon tannin sorbing material of certain mass, soaked 24 hours, place the CuSO of certain initial concentration then with deionized water
4In the solution, the pH value of regulator solution is 6.0, adopts sonic oscillation, and the chromatographic analysis post of packing into then adopts the mode of adorning column packing, Static Adsorption;
3, with spectrophotometric instrumentation process adsorbed solution absorbance, copper calibration curve and concentration-absorbance fit equation through having made can obtain CuSO
4Concentration after solution is adsorbed can get cattle-hide collagen fibers curing persimmon tannin to Cu through calculating
2+Adsorption rate;
4, adopt the H of 0.01mol/L
2SO
4Solution carries out desorb, and adsorbent that will be after desorb is Adsorption of Cu once more
2+The time, its absorption property is constant basically.
Embodiment 2
Get prepared cattle-hide collagen fibers and solidify persimmon tannin 0.5g, soaked 24 hours with deionized water, configuration contains Fe
2+Ion concentration is the FeSO of 1000mg/L
4Solution 50ml will solidify the persimmon tannin adsorbent and place FeSO
4In the solution, surveying its pH is 4.05, with the solution chromatographic analysis post of packing into, tightens glass piston, and vibration absorption was left standstill 48 hours after 4 hours; According to the Fe that adopts AAS to record
2+Calibration curve and fit equation Y=2.77556E-17+0.1915X calculate its absorption back concentration.Record: absorption back solution absorbency 0.008, corresponding concentration is 0.042mg/L, solidifies persimmon tannin to Fe through calculating this cattle-hide collagen fibers
2+Adsorption rate is 99.9%, has all adsorbed basically.
Adopted the H of 0.1mol/L
2SO
4Solution is to the adsorbent desorb, and effect is obvious, and it is the pale brown look before adsorbing that the adsorbent of absorption back black in color becomes again, and AAS records after the desorb Fe in the solution
2+The amount of ion is constant basically.
Embodiment 3
Get prepared cattle-hide collagen fibers and solidify persimmon tannin 0.5g, soaked 24 hours with deionized water, configuration contains Fe
3+Ion concentration is the Fe of 500mg/L
2(SO
4)
3Solution 50ml will solidify the persimmon tannin adsorbent and place Fe
2(SO
4)
3In the solution, surveying its pH is 2.18, with the solution chromatographic analysis post of packing into, tightens glass piston, and vibration absorption was left standstill 24 hours after 4 hours; According to the Fe that adopts AAS to record
3+Calibration curve and fit equation Y=0.01795+3.03771X calculate its absorption back concentration.Record: absorption back solution absorbency 0.147, corresponding concentration is 0.042mg/ml, solidifies persimmon tannin to Fe through calculating this cattle-hide collagen fibers
3+Adsorption rate is 91.5%, and adsorption capacity is 45.752mg/g; With solution after the absorption that has leached altogether among the 50ml, get wherein the 40ml chromatographic analysis post that continues to pack into, done adsorption test for the second time; After leaving standstill 24 hours once more, recording absorbance is 0.070, is 0.017mg/g according to its corresponding concentration of calibration curve fit equation; The result shows: after the absorption, concentration still reduces to some extent for the second time, shows that the process of solidifying the persimmon tannin adsorbing metal ions receives time effects; And the fastest at initial adsorption rate, increase in time, absorption tends to balance.
Adopted the H of 0.1mol/L
2SO
4Solution is to the adsorbent desorb, and effect is obvious, and it is the pale brown look before adsorbing that the adsorbent of absorption back black in color becomes again, and AAS records after the desorb Fe in the solution
3+The amount of ion is constant basically.
Embodiment 4
Get prepared cattle-hide collagen fibers and solidify persimmon tannin 0.5g, soaked 24 hours, put into the 50ml Cr of configuration with deionized water
6+Concentration is the K of 50mg/L
2CrO
4Solution, with the pH to 2.0 of the HCl regulator solution of 1.0mol/L, vibration absorption was left standstill 24 hours after 4 hours, according to the Cr that adopts AAS to record
6+Calibration curve and fit equation Y=-0.00154+0.5227X calculate its absorption back concentration.Record: absorption back solution absorbency is 0.012, and corresponding concentration is 0.079mg/L, solidifies persimmon tannin to Cr through calculating this cattle-hide collagen fibers
6+Adsorption rate is 99.95%.
The HCl solution that has adopted 5mol/L is to the adsorbent desorb, and effect is obvious, and it is the pale brown look before adsorbing that the adsorbent of absorption back black in color becomes again, and AAS records after the desorb Cr in the solution
6+The amount of ion is constant basically.
Embodiment 5
Get prepared cattle-hide collagen fibers and solidify persimmon tannin 0.2g, soaked 24 hours, put into the 50ml Cd of configuration with deionized water
2+Concentration is the CdSO of 100mg/L
4Solution, with the pH to 3.0 of the HCl regulator solution of 1.0mol/L, vibration absorption was left standstill 24 hours after 4 hours, according to the Cd that adopts AAS to record
2+Calibration curve and fit equation Y=0.3124X-0.0032 calculate its absorption back concentration.Record: absorption back solution absorbency is 0.018, and corresponding concentration is 0.0678mg/L, solidifies persimmon tannin to Cd through calculating this cattle-hide collagen fibers
2+Adsorption rate is 99.93%.
The ammoniacal liquor of HCl and 0.1mol/L of EDTA, 0.1mol/L that has adopted 0.02mol/L is to the adsorbent desorb, and it is the pale brown look before adsorbing that the adsorbent of absorption back black in color becomes again, and AAS records after the desorb Cd in the solution
2+The amount of ion is constant basically.
Claims (2)
1. the method for a persimmon tannin sorbing material absorption recovery heavy metal is characterized in that: comprise the steps:
(1) certain heavy metal solution of 5 groups of variable concentrations of configuration is made the calibration curve of heavy metal with spectrophotometer, and obtains its concentration-absorbance fit equation, degree of fitting R through linear fit
2Greater than 0.999;
(2) get the prepared cattle-hide collagen fibers of certain mass and solidify the persimmon tannin sorbing material; Soaked 24 hours with deionized water, place the heavy metal solution of step (1) initial concentration then, the pH value of regulator solution is 4.0～6.0; Adopt sonic oscillation; The chromatographic analysis post of packing into then adopts the mode of dress column packing, Static Adsorption;
(3) with spectrophotometric instrumentation process adsorbed solution absorbance; Through certain heavy metal calibration curve and the concentration-absorbance fit equation of having made; The concentration after certain heavy metal solution is adsorbed can be obtained, the adsorption rate of cattle-hide collagen fibers curing persimmon tannin sorbing material can be got certain heavy metal through calculating;
(4) adopt the strong acid solution of 0.01mol/L to carry out desorb, when will the adsorbent after desorb adsorbing heavy metal once more, its absorption property is constant basically.
2. method according to claim 1 is characterized in that: described cattle-hide collagen fibers solidified tannin adsorptive material, adopt the following steps preparation:
(1) takes by weighing 2 ~ 5 parts of the cattle-hide collagen fibers handled and 5 ~ 8 parts of persimmon powders, join mixed dissolution in the distilled water, stirred at normal temperatures 10 ~ 20 hours;
(2) add 3 ~ 8 parts of crosslinking agents, the pH of mixed solution is adjusted to 6.0 ~ 6.6, reacted at normal temperatures 1 ~ 3 hour with NaOH or the HCl aqueous solution; Crosslinking agent can be glutaraldehyde or formaldehyde;
(3) reacted product is put in the there-necked flask, 50 ~ 60 ℃ of following water-baths 3 ~ 5 hours;
(4) take out filtration, 60 ℃ of following vacuum drying; Taking-up is ground into fine powder with pulverizer, obtains collagen fiber solidified persimmon tannin sorbing material.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102925683A (en) * | 2012-11-05 | 2013-02-13 | 桂林电子科技大学 | Indium-iron separation method by using persimmontannin |
| CN104445499A (en) * | 2014-11-18 | 2015-03-25 | 华中农业大学 | Method for adsorbing and recycling heavy metal cadmium by using metal adsorbent employing persimmon leaves as raw material |
| CN105727907A (en) * | 2016-04-12 | 2016-07-06 | 桂林电子科技大学 | Magnetic persimmon tannin composite adsorption material and preparing method thereof |
| CN105921132A (en) * | 2016-07-11 | 2016-09-07 | 李旭颖 | Method for producing adsorbent by utilizing red bayberry processing byproducts |
| CN106957077A (en) * | 2017-04-25 | 2017-07-18 | 桂林电子科技大学 | A kind of processing method of Chemical Copper Plating Effluent |
| CN108031450A (en) * | 2017-11-15 | 2018-05-15 | 四川大学 | A kind of solidified tannin polyamide miillpore filter and its preparation method and application |
| CN111229173A (en) * | 2020-03-10 | 2020-06-05 | 四川大学 | Aminated collagen fiber adsorbing material and preparation method and application thereof |
| CN112473627A (en) * | 2020-10-19 | 2021-03-12 | 西北农林科技大学 | Tannin composite adsorbent and preparation method thereof |
| CN113000031A (en) * | 2021-03-31 | 2021-06-22 | 陕西科技大学 | Zinc oxide/collagen fiber composite porous adsorption material and preparation method and application thereof |
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| US4769223A (en) * | 1987-04-22 | 1988-09-06 | Bohumil Volesky | Biosorbent for gold |
| CN1410157A (en) * | 2002-11-27 | 2003-04-16 | 四川大学 | Collagen fiber solidified tannin adsorptive material and its preparation method and its adsorption and separation of metallic ion |
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| US4769223A (en) * | 1987-04-22 | 1988-09-06 | Bohumil Volesky | Biosorbent for gold |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102925683A (en) * | 2012-11-05 | 2013-02-13 | 桂林电子科技大学 | Indium-iron separation method by using persimmontannin |
| CN102925683B (en) * | 2012-11-05 | 2013-11-06 | 桂林电子科技大学 | Indium-iron separation method by using persimmontannin |
| CN104445499A (en) * | 2014-11-18 | 2015-03-25 | 华中农业大学 | Method for adsorbing and recycling heavy metal cadmium by using metal adsorbent employing persimmon leaves as raw material |
| CN105727907A (en) * | 2016-04-12 | 2016-07-06 | 桂林电子科技大学 | Magnetic persimmon tannin composite adsorption material and preparing method thereof |
| CN105727907B (en) * | 2016-04-12 | 2018-06-08 | 桂林电子科技大学 | A kind of magnetism persimmon tannin composite adsorbing material and preparation method thereof |
| CN105921132A (en) * | 2016-07-11 | 2016-09-07 | 李旭颖 | Method for producing adsorbent by utilizing red bayberry processing byproducts |
| CN106957077A (en) * | 2017-04-25 | 2017-07-18 | 桂林电子科技大学 | A kind of processing method of Chemical Copper Plating Effluent |
| CN108031450A (en) * | 2017-11-15 | 2018-05-15 | 四川大学 | A kind of solidified tannin polyamide miillpore filter and its preparation method and application |
| CN111229173A (en) * | 2020-03-10 | 2020-06-05 | 四川大学 | Aminated collagen fiber adsorbing material and preparation method and application thereof |
| CN112473627A (en) * | 2020-10-19 | 2021-03-12 | 西北农林科技大学 | Tannin composite adsorbent and preparation method thereof |
| CN113000031A (en) * | 2021-03-31 | 2021-06-22 | 陕西科技大学 | Zinc oxide/collagen fiber composite porous adsorption material and preparation method and application thereof |
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Application publication date: 20120704 |