CN102531083B - Method for treating aureomycin waste water with iron-modified attapulgite adsorbent - Google Patents

Method for treating aureomycin waste water with iron-modified attapulgite adsorbent Download PDF

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CN102531083B
CN102531083B CN201010582338.4A CN201010582338A CN102531083B CN 102531083 B CN102531083 B CN 102531083B CN 201010582338 A CN201010582338 A CN 201010582338A CN 102531083 B CN102531083 B CN 102531083B
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modified attapulgite
duomycin
attapulgite adsorbent
concentration
iron modified
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CN102531083A (en
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王金生
李剑
鲍文菊
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Beijing Normal University
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Beijing Normal University
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Abstract

The invention relates to a method for treating aureomycin waste water with an iron-modified attapulgite adsorbent, which is characterized in that concentration of aureomycin in the waste water is 5-150mg/L. The iron-modified attapulgite adsorbent is added in the aureomycin waste water, and mass ratio of the aureomycin waste water to the adsorbent is 1: (4-6). The adsorption process adopts a static mode of action and/or an oscillating and stirring mode of action at the temperature of 0-50 DEG C. The method aims at the waste water polluted by aureomycin and removes aureomycin by adding the iron-modified attapulgite adsorbent in the waste water for adsorption. The method has the advantages of having high adsorption efficiency for aureomycin compounds, simple operational process, low requirements for adsorption conditions, low cost of adsorption materials and high regeneration efficiency and being easy to popularize. The method is used for removing aureomycin compounds in a water body and has good economic and environmental benefits.

Description

A kind of iron modified attapulgite adsorbent is processed the method for duomycin waste water
Technical field
The present invention relates to the adsorption treatment method of duomycin compound in a kind of waste water, particularly relate to and utilize iron modified attapulgite adsorbent duomycin compound in medical sewage to be carried out to the method for Adsorption.
Background technology
Tetracycline antibiotics (tetracycline antibiotics, TCs, hereinafter to be referred as tetracyclines) is the class Broad spectrum antibiotics being produced by streptomycete, and frequency of utilization is high, scope is wide.It is reported, this type of production of antibiotics and usage quantity world rankings the second, China ranks the first.Tetracyclines comprises natural tetracyclines and semi-synthetic tetracyclines, and natural tetracyclines is to extract from Streptomyces nutrient solution, and duomycin (Aureomycin is called again Uromycin) is the one of natural tetracyclines.
China since early 1990s, duomycin widespread use in the industries such as medicine, livestock industry and aquaculture, its output and consumption are always in rising trend.But its production in above-mentioned industry and use and a large amount of waste water of producing are unprocessed or process and thoroughly do not make duomycin enter ecotope with water, therefore, the content of duomycin in water surrounding grows with each passing day, and the negative effect of the mankind and ecotope is also highlighted day by day.。
For the ecosystem, abuse duomycin can directly cause individual resistance.More and more data shows simultaneously, and more natural bacteriums are more much higher than what expect to the resistance of duomycin, and the drug resistance gene of bacterium may transfer occur at occurring in nature.The resistance of duomycin may pass to malignant bacteria from non-pathogenic bacteria, even may further propagate, and develops into the resistance on ecological level, and makes the individuality that does not directly touch duomycin also produce resistance.
Residual composition and the activity that can affect microorganisms in water of duomycin in water surrounding, thus microbial ecological structure changed, affect nitrated, the mineralization of soil and Nutrient Cycling of soil etc.In addition, the residual meeting of duomycin impacts plant, hydrobiont and soil organisms, because the difference of residual concentration produces harm such as suppressing growth or variation and teratogenesis.Because duomycin compound can be through the lipophilic group of cytolemma, and there is higher stability, therefore, be easy to biological accumulation and in environment long-term stable existence etc., thereby toxicity and the hazardness of aggravating it.
For reducing the ecological risk of duomycin compound in water surrounding, need to remove the duomycin compound in sewage or high density surface water body.Conventional water treatment method has at present: the combination treatment method of physics, chemistry and biological process and aforesaid method, but due to duomycin compound structure complexity, its toxicity and resistance concentration can affect the effect of biochemical treatment, and the conventional water treatment process of Sewage Plant is difficult to its removal.Compared with the complicated technology such as various advanced oxidations, catalyzed oxidation, absorbing process has the advantages such as technique is simple, treatment effect stable, relative low price.
Conventional sorbing material has gac, active sludge, clay class etc., gac is a kind of high-performance sorbing material, patent publication No. CN101333011 has introduced a kind of method of utilizing tsiklomitsin in mesoporous carbon Adsorption water, patent publication No. CN101337706 utilizes Powdered Activated Carbon to process the method for water body containing tetracycline antibiotics, two kinds of methods all have higher eliminating rate of absorption to tetracycline compound, absolutely proved the high absorption property of gac, but both are not all aimed at, duomycin compound studies, and this sorbing material preparation cost is higher, the economic situation current according to China, can not be widely used.Active sludge is the conventional treatment process of sewage work, but activated sludge process can not thoroughly be removed duomycin compound, along with the increase of underwater gold mycin concentration, eliminating rate of absorption reduces and treating processes has drug-fast microorganism in a large number by generation, will form potentially dangerous after entering environment.Therefore, it is very necessary developing a kind of novel, cheap clay class sorbing material, at present both at home and abroad about the absorption research of duomycin is fewer, there is report to adopt natural soil sorbing material to adsorb research as moisture soil, yellowish soil, rice soil, red soil etc., but natural soil sorbing material exists loading capacity low, adsorption concentration is limited in scope, and is not suitable for removing the duomycin compound in high density water body.
Attapulgite is a kind of natural clay mineral, owing to having unique layer chain crystalline structure and very tiny ((internal surface area can be up to 300-400m for bar-shaped, fibrous crystals form m) of approximately 0.01 μ m × 1 μ and larger specific surface area 2/ g, and outer surface area depends on the size of attapulgite crystal grain, according to actual measurement, Soviet Union's Anhui attapulgite outer surface area is about 23m 2/ g), determined that it has good absorption property.According to existing bibliographical information attapulgite, be heavy metal and organic strong sorbing material, and processing costs is only the 5-10% of gac, and regenerative operation is simple, and regeneration rate is high, the non-metal kind clay mineral that belongs to a kind of efficient, economy, environmental protection class, has broad prospect of application.Current document has been reported the removal of attapulgite to COD of sewage, and clearance can be up to more than 90%, and what have even reaches 100%, and regeneration rate is high, reusable, but the Adsorption that attapulgite is applied to duomycin compound is not appeared in the newspapers.
Summary of the invention
The object of this invention is to provide the method for duomycin compound in a kind of economy, the waste water of iron modified attapulgite adsorbent absorption efficiently.
Iron modified attapulgite adsorbent of the present invention is processed the method for duomycin waste water, it is characterized in that:
The concentration of described duomycin in waste water is 5-150mg/L;
At described duomycin waste water, add iron modified attapulgite adsorbent, the mass ratio of described duomycin waste water and described sorbent material is 1: (4-6), and preferably 1: 5.
Described adsorption process in temperature is under the condition of 0-50 ℃, adopt static state and/or vibration, stirring action mode is carried out.
In concrete enforcement,
The pH value scope of described duomycin waste water is 3-7.
Described adsorption time is 1-24h.
The method of described iron modified attapulgite adsorbent processing duomycin waste water also comprises the regeneration of sorbent material;
The regeneration of described sorbent material be by the saturated sorbent material of absorption mix with NaOH, immersion, clear water wash, wherein
Described NaOH concentration is 5%-15%, preferably 15%;
Described soak time is 2-3h.
Iron modified attapulgite adsorbent of the present invention is a kind of novel absorption material generating for the modification of attapulgite raw ore, and this material is higher to the adsorption efficiency of duomycin, after regeneration, can reuse, and economy is strong, simple to operate.
The preparation process of described iron modified attapulgite adsorbent is:
(1) attapulgite is purified
A. former attapulgite pulverizing, grinding are obtained to particle diameter≤100 object powder;
B. in concave and convex rod stone powder, add water, be made into the suspension that concentration is 5-10wt%, stir, concave and convex rod stone powder is uniformly dispersed;
C. in the suspension after dispersion treatment, add Sodium hexametaphosphate 99, the mass ratio of itself and attapulgite is 1-5: 100, stir 0.5h, and ultrasonic 1h, standing 2h, dewaters to mud cake shape, and 105 ℃ of dry 3h, obtain Concavo-convex stick after purifying stone;
(2) Concavo-convex and excellent after purifying stone modification
A. will in 5g Concavo-convex stick after purifying stone, add 150-200mL water, stir, Concavo-convex stick after purifying stone powder is uniformly dispersed,
B. add the FeCl of 0.2-5.0g 36H 2o,
C. add the HCl of appropriate 1mol/L or the NaOH of 1mol/L that pH value is adjusted to neutrality,
D. magnetic agitation 2-3h, centrifuge washing 2-3 time, dries 36-48h for 40 ℃, grinds and obtains particle diameter≤100 object iron modified attapulgite adsorbent.
Described absorption is subject to the molecular structure feature limits of duomycin own, and duomycin, under acid, alkali condition, reaction of degeneration all easily occurs, and known pH value value has material impact to absorption, experimental results show that the preferred pH value of duomycin solution scope is 3-7.It is little that absorption is affected by temperature, hunting speed, can select according to practical situation, and adsorbing the preferred time is 1-24h, and adsorption effect increases along with the growth of time, after absorption 24h, reaches adsorption equilibrium completely, and after balance, eliminating rate of absorption approaches 99%.
Described iron modified attapulgite regeneration, NaOH concentration is 5%-15%, and preferably NaOH concentration is 15%, soaks 2-3h, after clear water washing, can continue on for duomycin in planar water, and after regeneration, eliminating rate of absorption reaches 86.9%.
The present invention is directed to the waste water that polluted by duomycin, by adding iron modified attapulgite adsorbent to carry out Adsorption in waste water, beneficial effect of the present invention:
1. the adsorption efficiency of pair duomycin compound is high,
2. operating process is simple,
3. adsorption conditions requirement is low,
4. sorbing material is with low cost, regeneration efficiency is high, be easy to popularization.
Therefore, the present invention is applied to and removes duomycin compound in water body and have good economy and environmental benefit.
Accompanying drawing explanation
The impact of Fig. 1 time on eliminating rate of absorption
The impact of Fig. 2 duomycin starting point concentration on eliminating rate of absorption
The impact of Fig. 3 temperature on eliminating rate of absorption
The impact of Fig. 4 oscillation rate on eliminating rate of absorption
The impact of Fig. 5 pH on eliminating rate of absorption
The impact of the different iron amount of Fig. 6 modified attapulgite adsorbent on eliminating rate of absorption
Embodiment
Below in conjunction with specific examples, invention is described in detail.Scope of the present invention is not limited with embodiment, but is limited by the scope of claim.
Embodiment
Embodiment 1
Take 5g Concavo-convex stick after purifying stone and be placed in 500mL beaker, add 250mL distilled water, after magnetic agitation 0.5h, add the FeCl of 0.724g 36H 2o (being equivalent to 0.15gFe), magnetic agitation 30min, guarantees FeCl 36H 2o dissolves completely, regulates pH value=7, continues stirring 1h, after centrifuge washing 3 times, in 40 ℃ of dry 36-48h, is ground to particle diameter≤100 order, makes iron modified attapulgite adsorbent.
Accurate weighing is through iron modified attapulgite adsorbent 0.1000g (± 0.0005g), be placed in 250mL tool plug Erlenmeyer flask, adding 20mL concentration is in the duomycin solution of 100mg/L, be placed in constant temperature oscillator, the rate oscillation of 150r/min at 25 ℃ of temperature, at 1h, 3h, 6h, 12h, 24h, get supernatant liquor and cross respectively the millipore filtration of 0.45 μ m, test residual chlortetracycline concentration by liquid chromatography, every group experiment arrange three parallel, result is with arithmetical mean value representation, and calculate standard deviation, guarantee measuring accuracy.As calculated, duomycin eliminating rate of absorption is respectively 84.8%, 96.1%, 98.3%, 98.9%, 98.9%.Accompanying drawing 1, the impact of time on eliminating rate of absorption.
Visible, be adsorbed on 1h clearance and approach 85%, growth in time, clearance increases gradually, and after adsorption equilibrium, clearance approaches 99%.Adsorbing the preferred time is 1-24h.
Embodiment 2
With embodiment 1, make iron modified attapulgite adsorbent.
Accurate weighing is through iron modified attapulgite adsorbent 0.1000g (± 0.0005g), be placed in 250mL tool plug Erlenmeyer flask, add that 20mL concentration is respectively 10,20,50, in the duomycin solution of 100mg/L, be placed in constant temperature oscillator, at 25 ℃ of temperature, the rate oscillation 24h of 150r/min is to adsorption equilibrium, get supernatant liquor and cross the millipore filtration of 0.45 μ m, test residual chlortetracycline concentration by liquid chromatography, every group experiment arrange three parallel, result is with arithmetical mean value representation, and calculate standard deviation, guarantee measuring accuracy.As calculated, duomycin eliminating rate of absorption is respectively 99.4%, 98.8%, 98.6%, 98.9%.Accompanying drawing 2, the impact of duomycin starting point concentration on eliminating rate of absorption.
Visible, iron modified attapulgite adsorbent has very high clearance to the duomycin polluted-water of 5-150mg/L concentration.
Embodiment 3
With embodiment 1, make iron modified attapulgite adsorbent.
Accurate weighing is through iron modified attapulgite adsorbent 0.1000g (± 0.0005g), be placed in 250mL tool plug Erlenmeyer flask, adding 20mL concentration is in the duomycin solution of 100mg/L, be placed in constant temperature oscillator, respectively at 5,15,25,40 ℃ of temperature the rate oscillation 24h of 150r/min to adsorption equilibrium, get supernatant liquor and cross the millipore filtration of 0.45 μ m, test residual chlortetracycline concentration by liquid chromatography, every group experiment arrange three parallel, result is with arithmetical mean value representation, and calculate standard deviation, guarantee measuring accuracy.As calculated, duomycin eliminating rate of absorption is respectively 98.4%, 98.8%, 98.9%, 99.3%.Accompanying drawing 3, the impact of temperature on eliminating rate of absorption.
Visible, iron modified attapulgite adsorbent ADSORPTION OF GOLD mycin compound temperature influence is little, is applicable to the removal that the 0-50 ℃ of water body duomycin under temperature condition pollutes.
Embodiment 4
With embodiment 1, make iron modified attapulgite adsorbent.
Accurate weighing is through iron modified attapulgite adsorbent 0.1000g (± 0.0005g), be placed in 250mL tool plug Erlenmeyer flask, adding 20mL concentration is in the duomycin solution of 100mg/L, be placed in constant temperature oscillator, at 25 ℃ of temperature, respectively with 0,50,100,150, the rate oscillation 24h of 200r/min is to adsorption equilibrium, get supernatant liquor and cross the millipore filtration of 0.45 μ m, test residual chlortetracycline concentration by liquid chromatography, every group experiment arrange three parallel, result is with arithmetical mean value representation, and calculates standard deviation, guarantees measuring accuracy.As calculated, duomycin eliminating rate of absorption is respectively 98.7%, 99.2%, 99.1%, 98.9%, 99.1%.Accompanying drawing 4, the impact of oscillation rate on eliminating rate of absorption.
Visible, the service requirements of iron modified attapulgite adsorbent ADSORPTION OF GOLD mycin compound is low, can directly add use.
Embodiment 5
With embodiment 1, make iron modified attapulgite adsorbent.
Accurate weighing is through iron modified attapulgite adsorbent 0.1000g (± 0.0005g), be placed in 250mL tool plug Erlenmeyer flask, adding 20mL concentration is in the duomycin solution of 100mg/L, regulator solution pH value is respectively 1,3,5,7,9 and is placed in constant temperature oscillator, at 25 ℃ of temperature, the rate oscillation 24h of 150r/min is to adsorption equilibrium, get supernatant liquor and cross the millipore filtration of 0.45 μ m, test residual chlortetracycline concentration by liquid chromatography, every group experiment arrange three parallel, result is with arithmetical mean value representation, and calculate standard deviation, guarantee measuring accuracy.As calculated, duomycin eliminating rate of absorption is respectively 75.0%, 98.9%, 98.0%, 88.9%, 83.4%.Accompanying drawing 5, the impact of pH on eliminating rate of absorption.
Visible, pH is larger to Adsorption Effect, and preferred solution pH value scope is 3-7.
Embodiment 6
Take 5g Concavo-convex stick after purifying stone and be placed in 500mL beaker, add 250mL distilled water, after magnetic agitation 0.5h, add respectively the FeCl of 0.241g, 0.483g, 0.724g, 1.207g, 2.414g, 3.620g 36H 2o (being equivalent to respectively 0.05g, 0.10g, 0.15g, 0.25g, 0.50g, 0.75gFe), magnetic agitation 30min, guarantees FeCl 36H 2o dissolves completely, regulates pH value=7, continues stirring 1h, after centrifuge washing 3 times, in 40 ℃ of dry 36-48h, is ground to particle diameter≤100 order, makes the iron modified attapulgite adsorbent of different iron amounts.
Accurate weighing is through iron modified attapulgite adsorbent 0.1000g (± 0.0005g) respectively, be placed in 250mL tool plug Erlenmeyer flask, adding 20mL concentration is in the duomycin solution of 100mg/L, be placed in constant temperature oscillator, at 25 ℃ of temperature, with the rate oscillation 24h of 150r/min to adsorption equilibrium, get supernatant liquor and cross the millipore filtration of 0.45 μ m, test residual chlortetracycline concentration by liquid chromatography, every group experiment arrange three parallel, result is with arithmetical mean value representation, and calculates standard deviation, guarantees measuring accuracy.As calculated, duomycin eliminating rate of absorption is respectively 98.2%, 98.7%, 98.9%, 98.2%, 95.5%, 95.7%.Accompanying drawing 6, the impact of different iron amount modified attapulgite adsorbents on eliminating rate of absorption.

Claims (2)

1. iron modified attapulgite adsorbent is processed a method for duomycin waste water, it is characterized in that:
The preparation process of described iron modified attapulgite adsorbent is:
Take 5g Concavo-convex stick after purifying stone and be placed in 500mL beaker, add 250mL distilled water, after magnetic agitation 0.5h, add the FeCl of 0.724g 36H 2o, magnetic agitation 30min, guarantees FeCl 36H 2o dissolves completely, regulates pH value=7, continues stirring 1h, after centrifuge washing 3 times, in 40 ℃ of dry 36-48h, is ground to particle diameter≤100 order, makes iron modified attapulgite adsorbent;
Accurate weighing is through iron modified attapulgite adsorbent 0.1000g ± 0.0005g, be placed in 250mL tool plug Erlenmeyer flask, adding 20mL concentration is in the duomycin solution of 100mg/L, be placed in constant temperature oscillator, the rate oscillation of 150r/min at 25 ℃ of temperature, at 1h, 3h, 6h, 12h, 24h, get supernatant liquor and cross respectively the millipore filtration of 0.45 μ m, test residual chlortetracycline concentration by liquid chromatography, every group experiment arrange three parallel, result is with arithmetical mean value representation, and calculate standard deviation, guarantee measuring accuracy;
Or
After making as mentioned above iron modified attapulgite adsorbent, accurate weighing is through iron modified attapulgite adsorbent 0.1000g ± 0.0005g, be placed in 250mL tool plug Erlenmeyer flask, add 20mL concentration to be respectively 10, 20, 50, in the duomycin solution of 100mg/L, be placed in constant temperature oscillator, at 25 ℃ of temperature, the rate oscillation 24h of 150r/min is to adsorption equilibrium, get supernatant liquor and cross the millipore filtration of 0.45 μ m, test residual chlortetracycline concentration by liquid chromatography, every group experiment arrange three parallel, result is with arithmetical mean value representation, and calculate standard deviation, guarantee measuring accuracy,
Or
After making as mentioned above iron modified attapulgite adsorbent, accurate weighing is through iron modified attapulgite adsorbent 0.1000g ± 0.0005g, be placed in 250mL tool plug Erlenmeyer flask, adding 20mL concentration is in the duomycin solution of 100mg/L, be placed in constant temperature oscillator, respectively 5, 15, 25, at 40 ℃ of temperature, the rate oscillation 24h of 150r/min is to adsorption equilibrium, get supernatant liquor and cross the millipore filtration of 0.45 μ m, test residual chlortetracycline concentration by liquid chromatography, every group experiment arrange three parallel, result is with arithmetical mean value representation, and calculate standard deviation, guarantee measuring accuracy,
Or
After making as mentioned above iron modified attapulgite adsorbent, accurate weighing is through iron modified attapulgite adsorbent 0.1000g ± 0.0005g, be placed in 250mL tool plug Erlenmeyer flask, adding 20mL concentration is in the duomycin solution of 100mg/L, be placed in constant temperature oscillator, at 25 ℃ of temperature, respectively with 0, 50, 100, 150, the rate oscillation 24h of 200r/min is to adsorption equilibrium, get supernatant liquor and cross the millipore filtration of 0.45 μ m, test residual chlortetracycline concentration by liquid chromatography, every group experiment arrange three parallel, result is with arithmetical mean value representation, and calculate standard deviation, guarantee measuring accuracy,
Or
After making as mentioned above iron modified attapulgite adsorbent, accurate weighing is through iron modified attapulgite adsorbent 0.1000g ± 0.0005g, be placed in 250mL tool plug Erlenmeyer flask, adding 20mL concentration is in the duomycin solution of 100mg/L, regulator solution pH value is respectively 1, 3, 5, 7, 9 are placed in constant temperature oscillator, at 25 ℃ of temperature, the rate oscillation 24h of 150r/min is to adsorption equilibrium, get supernatant liquor and cross the millipore filtration of 0.45 μ m, test residual chlortetracycline concentration by liquid chromatography, every group experiment arrange three parallel, result is with arithmetical mean value representation, and calculate standard deviation, guarantee measuring accuracy,
Or adopt following methods to make the iron modified attapulgite adsorbent of different iron amounts:
Take 5g Concavo-convex stick after purifying stone and be placed in 500mL beaker, add 250mL distilled water, after magnetic agitation 0.5h, add respectively the FeCl of 0.241g, 0.483g, 0.724g, 1.207g, 2.414g, 3.620g 36H 2o, magnetic agitation 30min, guarantees FeCl 36H 2o dissolves completely, regulates pH value=7, continues stirring 1h, after centrifuge washing 3 times, in 40 ℃ of dry 36-48h, is ground to particle diameter≤100 order, makes the iron modified attapulgite adsorbent of different iron amounts;
Accurate weighing is through iron modified attapulgite adsorbent 0.1000g ± 0.0005g respectively, be placed in 250mL tool plug Erlenmeyer flask, adding 20mL concentration is in the duomycin solution of 100mg/L, be placed in constant temperature oscillator, at 25 ℃ of temperature, with the rate oscillation 24h of 150r/min to adsorption equilibrium, get supernatant liquor and cross the millipore filtration of 0.45 μ m, test residual chlortetracycline concentration by liquid chromatography, every group experiment arrange three parallel, result is with arithmetical mean value representation, and calculates standard deviation, guarantees measuring accuracy;
The method of described iron modified attapulgite adsorbent processing duomycin waste water also comprises the regeneration of sorbent material;
The regeneration of described sorbent material be by the saturated sorbent material of absorption mix with NaOH, immersion, clear water wash, wherein
Described NaOH concentration is 5%-15%; Described soak time is 2-3h.
2. iron modified attapulgite adsorbent as claimed in claim 1 is processed the method for duomycin waste water, it is characterized in that:
Described NaOH concentration is 15%.
CN201010582338.4A 2010-12-10 2010-12-10 Method for treating aureomycin waste water with iron-modified attapulgite adsorbent Expired - Fee Related CN102531083B (en)

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