CN109395700A - A kind of method of cadmium in compound microalgae biological adsorption agent and its adsorbent absorption waste water - Google Patents
A kind of method of cadmium in compound microalgae biological adsorption agent and its adsorbent absorption waste water Download PDFInfo
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Abstract
The present invention relates to a kind of methods of cadmium in sewage treatment field more particularly to compound microalgae biological adsorption agent and its adsorbent absorption waste water.It overcomes in the processing of microalgae absorption Pollutants in Wastewater in the prior art, microalgae is easy to be lost from reactor, and the separating difficulty of microalgae and waste water is big after the completion of processing, problem at high cost, activity of microalgae is lower, by chlorella cells elder generation and Fe3O4Nanoparticle carries out absorption connection, then carries out mixing embedding fixation with sodium alginate again, prepares compound microalgae biological adsorption agent, which has many advantages, such as that adsorption capacity is big, the rate of adsorption is fast, simple to operate, and includes magnetic Fe3O4Nanoparticle can facilitate the quick recycling for realizing adsorbent after having handled waste water.The compound microalgae biological adsorption agent is used for the Adsorption of heavy metal ions in wastewater cadmium (Cd), achieves good removal effect.
Description
Technical field
The present invention relates to sewage treatment fields more particularly to a kind of compound microalgae biological adsorption agent and its adsorbent to adsorb
The method of cadmium in waste water.
Background technique
Cadmium (Cd) is widely used in the fields such as electroplating industry, chemical industry, electronics industry and nuclear industry as a kind of metal, every year
There are a considerable amount of cadmiums (Cd) to be discharged into environment by exhaust gas, waste water, waste residue, pollutes.Compared to other metals, cadmium is easier
It is absorbed by crops, to form huge threat to human health.
Common cadmium (Cd) processing method has the methods of chemical precipitation method, ion-exchange, absorption method.Absorption method is for giving up
The removal of heavy metal contaminants is flexible and convenient with operating process in water, is able to achieve advanced treating, recycles waste water by energy of desorption
In heavy metal ion the advantages that, be widely used in the processing of all kinds of heavy metal wastewater therebies.
Chlorella as a kind of microalgae have growth rate it is fast, the low advantage of toxigenic capacity, and can effectively adsorb and
The some metal ions being enriched in water, are a kind of efficient living body biological adsorbents.It is polluted in traditional microalgae absorption waste water
In the processing of object, microalgae is generally in the state of suspension growth, be easy be lost from reactor, and handle after the completion of microalgae with
The separation of waste water brings biggish operating cost, and the microalgae of suspension growth is weaker to the resistance of toxicant, in waste water
Under the action of the pollutants such as middle heavy metal, activity is often difficult to maintain, and causes whole treatment effeciency lower.
Such as a kind of a kind of method for Immobilized cells culture processing breeding wastewater reported in Chinese patent literature, it is open
Number be CN108424906A, with chlorella to the absorption and utilization of nutriment in waste water and other microelements and seaweed
The immobilization role of sour sodium makes chlorella can be good at carrying out the separation of algae water while playing catharsis to waste water.We
The advantages of method be with Immobilization in Sodium Alginate chlorella handle aquiculture waste water, alleviate increasingly serious fresh water pressure；
And absorption and utilization of the chlorella to various elements in waste water, it is purified waste water, and then slow down it and be ultimately discharged into
The load of natural water.But there is also shortcomings, such as its recycling is more difficult, needs by constantly filtering
It can be realized, the separation of algae water, separating difficulty is larger.
Summary of the invention
The present invention is to overcome in the processing of microalgae absorption Pollutants in Wastewater in the prior art, and microalgae is easy from reaction
It is lost in device, the separating difficulty of microalgae and waste water is big after the completion of processing, and problem at high cost, activity of microalgae is lower provides one
Kind can effectively fix microalgae, prevent microalgae to be lost from reactor, the convenient separation of microalgae and waste water, micro- after the completion of processing
The method of cadmium in a kind of high compound microalgae biological adsorption agent of algae activity and its adsorbent absorption waste water.
For achieving the above object, the invention is realized by the following technical scheme:
A kind of compound microalgae biological adsorption agent, the compound microalgae biological adsorption agent the preparation method is as follows:
(S.1) chlorella is cultivated: chlorella being cultivated in the medium, medium centrifugal separation obtains lower layer's concentration
Microalgae biology；
(S.2) magnetic particle compounds: the microalgae biology dilution of concentration, and and magnetic Fe3O4Nanoparticle is compounded, and is completed micro-
Frustule and magnetic Fe3O4Absorption between nanoparticle is fixed；
(S.3) prepared by immobilized microspheres: sodium alginate being added in Xiang Shangshu solution, is then added drop-wise to CaCl2In solution, prepare
Immobilized microspheres, i.e., compound microalgae biological adsorption agent.
Microalgae biological adsorption agent in the present invention its by by microalgae and Fe3O4Compounded between nanoparticle, by its two
Person carries out absorption connection, so that microalgae adsorption has Fe3O4Nanoparticle so that microalgae its have magnetism, then again will
It is immobilized, and prepares immobilized microspheres, can prevent the suspension growth of microalgae, solves traditional microalgae absorption waste water
In the processing of middle pollutant, microalgae is generally in the state of suspension growth, is easy the problem of being lost from reactor.Meanwhile it passing
The microalgae of suspension growth is weaker to the resistance of toxicant in system method, under the action of the pollutants such as heavy metal in waste water,
Its activity is often difficult to maintain, and causes whole treatment effeciency lower, its resistance to toxicant after being fixed
Effectively enhancing, improves whole treatment effeciency.It, just can be effective by magnetic-adsorption meanwhile after the completion of sewage treatment
Promotion is adsorbed, thus effective pair of separation sewage and microalgae.
Preferably, culture medium is BG11 culture medium in the step (S.1), the centrifugation rate is 3000-
5000rpm, centrifugation time 5-10min.
Preferably, being diluted using sterile water to the microalgae biology of concentration in the step (S.2), concentration is adjusted
The OD of liquid680For 1-1.5.
As the OD of concentrate680Value is in this interval range, and activity is higher, therefore its suction to heavy metal in sewage
Attached performance activity with higher.
Preferably, magnetic Fe in the step (S.2)3O4Nanoparticle the preparation method is as follows: using FeCl3、
FeSO4Acidic iron salt solutions are prepared with hydrochloric acid, make Fe3+、Fe2+Molar ratio with HCl is (1.0-2.5): 1:1, which is dripped
It is added in the ammonium hydroxide that mass fraction is 20%-30%, the volume ratio of iron salt solutions and ammonium hydroxide is 1:3-1:5, is stirred evenly, wait produce
After object color becomes brown, magnetic separation is staticly settled and carried out, extra liquid is gone, the precipitating of bottom is sucked simultaneously with magnet
Distilled water is added to clean 3-4 times, filtering obtains Fe3O4, through 36~72h of vacuum freeze drying, it is prepared into magnetic Fe3O4Nanoparticle
Son.
Magnetic Fe in the present invention3O4Nanoparticle passes through Fe3+、Fe2+Between compounding, then will be obtained by ammonia precipitation process
To Fe3O4Nanoparticle, with good magnetism, so that can be reduced by magnetic-adsorption after microalgae absorption is fixed
The difficulty that microalgae is separated with waste water.
Preferably, magnetic Fe in the step (S.2)3O4The additive amount of nanoparticle is to add magnetic in every liter of algae solution
Property Fe3O40.2~0.4g of nanoparticle.
Preferably, compounding condition is isothermal vibration 2-4 days in the step (S.2).
Preferably, the mass fraction concentration of sodium alginate is 5%-7%, CaCl in the step (S.3)2Solution
Mass concentration is 3.5%.
Preferably, in the step (S.3), the diameter of immobilized microspheres obtained is 2-5mm, in immobilized microspheres
Biomass containing microalgae is 1.0 × 109-6.0×109cell/g。
The diameter of immobilized microspheres in the present invention is smaller, thus the life of specific surface area with higher and higher concentration
Object amount, so as to promote the efficiency of pollutant in absorption effluent.
A method of if preceding resulting compound microalgae biological adsorption agent adsorbs cadmium in waste water, the method is as follows:
The compound microalgae biological adsorption agent is added in cadmium wastewater, the removal of cadmium in waste water is completed in concussion absorption, after the completion of absorption
Quick magnetic separation is carried out to the microalgae biological adsorption agent in waste water.
Compound microalgae biological adsorption agent in the present invention is after having adsorbed the cadmium element in water, it is thus only necessary to pass through magnetic force
Separation can separate sewage with compound microalgae biological adsorption agent, have the characteristics that high-efficient simple, to reduce separation
Cost.
Preferably, the concentration of cadmium is 2-20mg/L, the throwing of compound microalgae biological adsorption agent in the cadmium wastewater
Dosage is 10-25g/L, and adsorption temp is 28-36 DEG C, pH value 6-9.
Therefore, the invention has the following advantages: the compound microalgae biological adsorption agent in (1) present invention can be effective
Fixed microalgae, prevents microalgae to be lost from reactor；(2) convenient separation of microalgae and waste water, separation costs are low after the completion of handling；
(3) microalgae resistance to poison is stronger, and activity is high, and disposed of in its entirety treatment effeciency is high.
Specific embodiment
The embodiment of technical solution of the present invention will be described in detail below.Following embodiment is only used for clearer
Ground illustrates technical solution of the present invention, therefore is only used as an example, and not intended to limit the protection scope of the present invention.
Compound microalgae biological adsorption agent
Embodiment 1
A kind of compound microalgae biological adsorption agent, the compound microalgae biological adsorption agent the preparation method is as follows:
(S.1) chlorella is cultivated: chlorella being cultivated in BG11 culture medium, culture solution is centrifugated at 4500rpm
7min obtains the microalgae biology of lower layer's concentration；
(S.2) magnetic particle compounds: the microalgae biology of concentration is diluted with sterile water, adjusts the OD of concentrate680It is 1.1, and and magnetic
Property Fe3O4Nanoparticle is compounded, and adds magnetic Fe in every liter of algae solution3O4Nanoparticle 0.35g, it is complete after isothermal vibration 2 days
At microalgae cell and magnetic Fe3O4Absorption between nanoparticle is fixed；
(S.3) prepared by immobilized microspheres: the sodium alginate that mass fraction concentration is 5.5% being added in Xiang Shangshu solution, then drips
It is added to the CaCl that mass concentration is 3.5%2In solution, preparing diameter is 4mm, the biomass containing microalgae in immobilized microspheres
It is 5.5 × 109The immobilized microspheres of cell/g, i.e., compound microalgae biological adsorption agent.
Magnetic Fe in the step (S.2)3O4Nanoparticle the preparation method is as follows: using FeCl3、FeSO4And hydrochloric acid
Acidic iron salt solutions are prepared, Fe is made3+、Fe2+Molar ratio with HCl is 1.0:1:1, which, which is added drop-wise to mass fraction, is
In 20% ammonium hydroxide, the volume ratio of iron salt solutions and ammonium hydroxide is 1:3, is stirred evenly, and after coloured product becomes brown, is staticly settled
And magnetic separation is carried out, extra liquid is gone, the precipitating of bottom is sucked with magnet and distilled water is added and cleans 3 times, is filtered
Obtain Fe3O4, through vacuum freeze drying 36h, it is prepared into magnetic Fe3O4Nanoparticle.
Embodiment 2
A kind of compound microalgae biological adsorption agent, the compound microalgae biological adsorption agent the preparation method is as follows:
(S.1) chlorella is cultivated: chlorella being cultivated in BG11 culture medium, culture solution is centrifugated at 3,000 rpm
5min obtains the microalgae biology of lower layer's concentration；
(S.2) magnetic particle compounds: the microalgae biology of concentration is diluted with sterile water, adjusts the OD of concentrate680Be 1, and with magnetism
Fe3O4Nanoparticle is compounded, and adds magnetic Fe in every liter of algae solution3O4Nanoparticle 0.2g after isothermal vibration 2 days, is completed micro-
Frustule and magnetic Fe3O4Absorption between nanoparticle is fixed；
(S.3) prepared by immobilized microspheres: the sodium alginate that mass fraction concentration is 5% being added in Xiang Shangshu solution, is then added dropwise
The CaCl for being 3.5% to mass concentration2In solution, preparing diameter is 2mm, and the biomass containing microalgae is in immobilized microspheres
1.0×109The immobilized microspheres of cell/g, i.e., compound microalgae biological adsorption agent.
Magnetic Fe in the step (S.2)3O4Nanoparticle the preparation method is as follows: using FeCl3、FeSO4And hydrochloric acid
Acidic iron salt solutions are prepared, Fe is made3+、Fe2+Molar ratio with HCl is 2.5:1:1, which, which is added drop-wise to mass fraction, is
In 30% ammonium hydroxide, the volume ratio of iron salt solutions and ammonium hydroxide is 1:5, is stirred evenly, and after coloured product becomes brown, is staticly settled
And magnetic separation is carried out, extra liquid is gone, the precipitating of bottom is sucked with magnet and distilled water is added and cleans 4 times, is filtered
Obtain Fe3O4, through vacuum freeze drying 72h, it is prepared into magnetic Fe3O4Nanoparticle.
Embodiment 3
A kind of compound microalgae biological adsorption agent, the compound microalgae biological adsorption agent the preparation method is as follows:
(S.1) chlorella is cultivated: chlorella being cultivated in BG11 culture medium, culture solution is centrifugated at 5000rpm
10min obtains the microalgae biology of lower layer's concentration；
(S.2) magnetic particle compounds: the microalgae biology of concentration is diluted with sterile water, adjusts the OD of concentrate680It is 1.5, and and magnetic
Property Fe3O4Nanoparticle is compounded, and adds magnetic Fe in every liter of algae solution3O4Nanoparticle 0.4g after isothermal vibration 4 days, is completed
Microalgae cell and magnetic Fe3O4Absorption between nanoparticle is fixed；
(S.3) prepared by immobilized microspheres: the sodium alginate that mass fraction concentration is 7% being added in Xiang Shangshu solution, is then added dropwise
The CaCl for being 3.5% to mass concentration2In solution, preparing diameter is 5mm, and the biomass containing microalgae is in immobilized microspheres
6.0×109The immobilized microspheres of cell/g, i.e., compound microalgae biological adsorption agent.
Magnetic Fe in the step (S.2)3O4Nanoparticle the preparation method is as follows: using FeCl3、FeSO4And hydrochloric acid
Acidic iron salt solutions are prepared, Fe is made3+、Fe2+Molar ratio with HCl is 1.5:1:1, which, which is added drop-wise to mass fraction, is
In 25% ammonium hydroxide, the volume ratio of iron salt solutions and ammonium hydroxide is 1:4, is stirred evenly, and after coloured product becomes brown, is staticly settled
And magnetic separation is carried out, extra liquid is gone, the precipitating of bottom is sucked with magnet and distilled water is added and cleans 3 times, is filtered
Obtain Fe3O4, through vacuum freeze drying 60h, it is prepared into magnetic Fe3O4Nanoparticle.
Embodiment 4
A kind of compound microalgae biological adsorption agent, the compound microalgae biological adsorption agent the preparation method is as follows:
(S.1) chlorella is cultivated: chlorella being cultivated in BG11 culture medium, culture solution is centrifugated at 4000rpm
8min obtains the microalgae biology of lower layer's concentration；
(S.2) magnetic particle compounds: the microalgae biology of concentration is diluted with sterile water, adjusts the OD of concentrate680It is 1.2, and and magnetic
Property Fe3O4Nanoparticle is compounded, and adds magnetic Fe in every liter of algae solution3O4Nanoparticle 0.3g after isothermal vibration 3 days, is completed
Microalgae cell and magnetic Fe3O4Absorption between nanoparticle is fixed；
(S.3) prepared by immobilized microspheres: the sodium alginate that mass fraction concentration is 6% being added in Xiang Shangshu solution, is then added dropwise
The CaCl for being 3.5% to mass concentration2In solution, preparing diameter is 3mm, and the biomass containing microalgae is in immobilized microspheres
5.0×109The immobilized microspheres of cell/g, i.e., compound microalgae biological adsorption agent.
Magnetic Fe in the step (S.2)3O4Nanoparticle the preparation method is as follows: using FeCl3、FeSO4And hydrochloric acid
Acidic iron salt solutions are prepared, Fe is made3+、Fe2+Molar ratio with HCl is 2:1:1, and it is 25% which, which is added drop-wise to mass fraction,
Ammonium hydroxide in, the volume ratio of iron salt solutions and ammonium hydroxide is 1:4, is stirred evenly, and after coloured product becomes brown, staticly settles and goes forward side by side
Row magnetic separation removes extra liquid, and the precipitating of bottom is sucked with magnet and distilled water is added and cleans 4 times, and filtering obtains
Fe3O4, through vacuum freeze drying 48h, it is prepared into magnetic Fe3O4Nanoparticle.
Embodiment 5
A kind of compound microalgae biological adsorption agent, the compound microalgae biological adsorption agent the preparation method is as follows:
(S.1) chlorella is cultivated: chlorella being cultivated in BG11 culture medium, culture solution is centrifugated at 3500rpm
6min obtains the microalgae biology of lower layer's concentration；
(S.2) magnetic particle compounds: the microalgae biology of concentration is diluted with sterile water, adjusts the OD of concentrate680It is 1.3, and and magnetic
Property Fe3O4Nanoparticle is compounded, and adds magnetic Fe in every liter of algae solution3O4Nanoparticle 0.35g, it is complete after isothermal vibration 3 days
At microalgae cell and magnetic Fe3O4Absorption between nanoparticle is fixed；
(S.3) prepared by immobilized microspheres: the sodium alginate that mass fraction concentration is 5%-7% being added in Xiang Shangshu solution, then
It is added drop-wise to the CaCl that mass concentration is 3.5%2In solution, preparing diameter is 4mm, the biology containing microalgae in immobilized microspheres
Amount is 4.0 × 109The immobilized microspheres of cell/g, i.e., compound microalgae biological adsorption agent.
Magnetic Fe in the step (S.2)3O4Nanoparticle the preparation method is as follows: using FeCl3、FeSO4And hydrochloric acid
Acidic iron salt solutions are prepared, Fe is made3+、Fe2+Molar ratio with HCl is 1.8:1:1, which, which is added drop-wise to mass fraction, is
In 28% ammonium hydroxide, the volume ratio of iron salt solutions and ammonium hydroxide is 1:5, is stirred evenly, and after coloured product becomes brown, is staticly settled
And magnetic separation is carried out, extra liquid is gone, the precipitating of bottom is sucked with magnet and distilled water is added and cleans 3 times, is filtered
Obtain Fe3O4, through vacuum freeze drying 70h, it is prepared into magnetic Fe3O4Nanoparticle.
The method of cadmium in compound microalgae biological adsorption agent absorption waste water
Embodiment 6
Compound microalgae biological adsorption agent obtained in embodiment 3 carries out it to test except cadmium, the method is as follows: this is compound
Microalgae biological adsorption agent is added containing in cadmium (Cd) waste water, and total cadmium (Cd) concentration is 2-20mg/L in suitable waste water, compound micro-
The dosage of algae biological adsorption agent: 10-25g/L (waste water), 28-36 DEG C of adsorption temp, pH is controlled in 6-9.It is adsorbed by concussion
The removal for completing cadmium (Cd) in waste water carries out quick magnetic separation to the microalgae biological adsorption agent in waste water after the completion of absorption, adopts
With cadmium (Cd) concentration total in atomic absorption spectroscopy determination waste water, removal rate is calculated, and is imitated with the absorption of suspension chlorella
Rate compares, and result is as shown in following table.
The adsorption efficiency of cadmium (Cd) under the different pH value of table 1
Cadmium in considerably higher waste water is achieved compared to suspension microalgae by the visible compound microalgae biological adsorption agent of data in table
(Cd) removal rate, and by significantly improving stability of the chlorella in terms of heavy metals removal after compound fixation, in pH
Good cadmium (Cd) Adsorption effect is achieved in the range of value 6-9.
Claims (10)
1. a kind of compound microalgae biological adsorption agent, which is characterized in that the preparation side of the compound microalgae biological adsorption agent
Method is as follows:
(S.1) chlorella is cultivated: chlorella being cultivated in the medium, medium centrifugal separation obtains lower layer's concentration
Microalgae biology；
(S.2) magnetic particle compounds: the microalgae biology dilution of concentration, and and magnetic Fe3O4Nanoparticle is compounded, and is completed micro-
Frustule and magnetic Fe3O4Absorption between nanoparticle is fixed；
(S.3) prepared by immobilized microspheres: then middle addition sodium alginate in Xiang Shangshu solution is added drop-wise to CaCl2In solution, preparation
Immobilized microspheres out, i.e., compound microalgae biological adsorption agent.
2. a kind of compound microalgae biological adsorption agent according to claim 1, which is characterized in that the step (S.1)
Middle culture medium is BG11 culture medium, and the centrifugation rate is 3000-5000 rpm, and centrifugation time is 5-10 min.
3. a kind of compound microalgae biological adsorption agent according to claim 1, which is characterized in that the step (S.2)
It is middle to be diluted using microalgae biology of the sterile water to concentration, adjust the OD of concentrate680For 1-1.5.
4. a kind of compound microalgae biological adsorption agent according to claim 1, which is characterized in that the step (S.2)
Middle magnetic Fe3O4Nanoparticle the preparation method is as follows: using FeCl3、FeSO4Acidic iron salt solutions are prepared with hydrochloric acid, make Fe3+、
Fe2+Molar ratio with HCl is (1.0-2.5): 1:1, which is added drop-wise in the ammonium hydroxide that mass fraction is 20%-30%, molysite
The volume ratio of solution and ammonium hydroxide is 1:3-1:5, is stirred evenly, and after coloured product becomes brown, staticly settles and carries out magnetic force point
From, extra liquid is gone, the precipitating of bottom is sucked with magnet and distilled water is added and cleans 3-4 times, filtering acquisition Fe3O4, warp
36 ~ 72 h of vacuum freeze drying, is prepared into magnetic Fe3O4Nanoparticle.
5. a kind of compound microalgae biological adsorption agent described according to claim 1 or 3 or 4, which is characterized in that the step
(S.2) magnetic Fe in3O4The additive amount of nanoparticle is to add magnetic Fe in every liter of algae solution3O40.2 ~ 0.4 g of nanoparticle.
6. a kind of compound microalgae biological adsorption agent described according to claim 1 or 3 or 4, which is characterized in that the step
(S.2) compounding condition is isothermal vibration 2-4 days in.
7. a kind of compound microalgae biological adsorption agent according to claim 1, which is characterized in that the step (S.3)
The mass fraction concentration of middle sodium alginate is 5%-7%, CaCl2The mass concentration of solution is 3.5%.
8. a kind of compound microalgae biological adsorption agent according to claim 1 or claim 7, which is characterized in that the step
(S.3) in, the diameter of immobilized microspheres obtained is 2-5 mm, and the biomass containing microalgae is 1.0 × 10 in immobilized microspheres9
-6.0×109cell/g。
9. the method for cadmium, feature in a kind of microalgae biological adsorption agent absorption waste water compound as obtained in claim 1 ~ 8
It is, the method is as follows: the compound microalgae biological adsorption agent is added in cadmium wastewater, concussion absorption is completed in waste water
The removal of cadmium carries out quick magnetic separation to the microalgae biological adsorption agent in waste water after the completion of absorption.
10. the method for cadmium in compound microalgae biological adsorption agent absorption waste water according to claim 9, which is characterized in that
The concentration of cadmium is 2-20 mg/L in the cadmium wastewater, and the dosage of compound microalgae biological adsorption agent is 10-25 g/L,
Adsorption temp is 28-36 DEG C, pH value 6-9.
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