CN106622167A - Heavy metal adsorption immobilized biological adsorbent and preparation method and application thereof - Google Patents
Heavy metal adsorption immobilized biological adsorbent and preparation method and application thereof Download PDFInfo
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
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Abstract
The invention discloses a heavy metal adsorption immobilized biological adsorbent and a preparation method thereof. The adsorbent is prepared from disposable foam meal boxes, pistia stratiotes powder, sodium alginate and polyvinyl alcohol in a mass ratio of 4:4:1:5. The disposable foam meal boxes, dried pistia stratiotes powder, sodium alginate and polyvinyl alcohol are adopted for preparing solid particles to obtain particles of the immobilized biological adsorbent. The immobilized biological adsorbent is a novel adsorbent which is low in cost, extensive in material source, great in adsorption effect and recyclable, and has a high application value in heavy metal wastewater treatment.
Description
Technical field
The present invention relates to heavy metal processing technology field, the immobilized biological adsorbent of specifically a kind of Adsorption of Heavy Metals and
Preparation Method And The Use.
Background technology
Traditional process for treating heavy-metal waste water has many deficiencies such as high cost, poisonous, generation secondary pollution, though
So recent domestic scholar has carried out technological transformation for the deficiency that these methods are present, and achieves certain achievement, such as grinds
New and effective precipitating reagent, curing agent, seperation film etc. are made, but still the most essential shortcoming of these methods presence cannot be overcome.It is raw
Thing adsorption technology is a new way in heavy metal containing wastewater treatment, abundant with raw material sources, wide in variety, adsorption plant letter
Single easy to operate, adsorption rate is fast, adsorbance is big, good selective, becomes current study hotspot both domestic and external.But, it is raw
Often density is little for the biomaterial that thing adsorption technology is adopted, low intensity, particle diameter are little, must be through heavy after Adsorption of Heavy Metals
Drop, filtration or centrifugation could separate it with solution, and adsorbent can be lost in practical operation, and solid-liquid after the completion of adsorbing
Separation is relatively complicated, and this process not only increases processing cost, and reduces removal efficiency.Therefore, by biological adsorption skill
Art pushes practical application to, it is necessary to change existence form so as to can be by convenient use as ion exchange resin or activated carbon.
Immobilization technology be using the area of space that physically or chemically material of free state is positioned at restriction by means simultaneously
Make its keep activity and can be with a kind of technology of Reusability.At present immobilization technology mainly has covalent coupling method, cross-linking method, bag
Combination of method and various process for fixation etc. is buried, wherein more universal with the application of investment.Fixation support has many kinds,
Conventional mainly has:Natural macromolecule amylose class, such as:Sodium alginate, gelatin etc.;Organic synthesis macromolecular material, such as polyethylene
Alcohol, polyacrylamide etc..Gel embedding method be material (such as plant powder) is embedded in the micropore inside gel material or
In the bead by made by various high molecular polymers.Investment making immobilized spherule is simple to operate, mild condition.Prior art
In, some application examples of investment immobilization technology in sewage disposal are had been disclosed for, such as:Dong Xinjiao et al. alginic acids
Calcium embedding branch spore it is mould after adsorption test research is carried out to Cu2+ in water, as a result find, when calcium alginate mass fraction be 3%,
When the mass fraction of CaCl2 is 4%, thalline fraction is 15%, the obtained immobilized spherule of embedding has preferable mechanicalness
Energy and higher adsorbance, biological adsorption equilibration time is 3h;Feature obtained in the polyvinyl alcohol immobilized free bacterium such as Gan Li
Biological bead, crystal violet (CV) and Cr (VI) that can simultaneously in Adsorption waste water from dyestuff, in 42h to CV (60mg/L) and Cr
(VI) clearance (50mg/L) is up to 92.7% and 25.9%;Ben Yue etc. fixes embedding verdigris using polyvinyl alcohol and sodium alginate
Microcystis aeruginosa prepares immobilized spherule, is 6~8 in solution ph, and it is 9~12d that absorption reaches the time of balance, and initial phosphorus concentration is
Clearance reaches 79.19% during 1.00mg/L.But in prior art, typically using polyvinyl alcohol or sodium alginate as immobilization
Carrier, the shaping particles effect prepared using polyvinyl alcohol or Immobilization in Sodium Alginate is poor, is easily sticked together, mechanical strength
It is not high;Time of equilibrium adsorption is more long, and time cost is high, and efficiency is low.It is broken in adsorption process, cause formation powder in water to be hanged
Float, affects effluent quality.
The content of the invention
It is an object of the invention to provide a kind of immobilized biological adsorbent of Adsorption of Heavy Metals and preparation method thereof and use
On the way, to solve the problems, such as above-mentioned background technology in propose.
For achieving the above object, the present invention provides following technical scheme:
A kind of immobilized biological adsorbent of Adsorption of Heavy Metals, by disposable foam cutlery box, great Piao powder, sodium alginate and
Polyvinyl alcohol is made.
As further scheme of the invention:The disposable foam cutlery box, great Piao powder, sodium alginate and polyvinyl alcohol
Mass ratio be 4:4:1:5.
As further scheme of the invention:The sodium alginate and polyvinyl alcohol are AR.
The preparation method of the immobilized biological adsorbent of the Adsorption of Heavy Metals, step is as follows:
1) after disposable foam cutlery box is shredded, in being dissolved in ethyl acetate, liquid A is obtained;
2) great Piao powder is added into liquid A, after stirring, obtains liquid B;
3) by sodium alginate and polyvinyl alcohol, and heating for dissolving is in water, obtains liquid C;
4) liquid C is added into liquid B, and is uniformly mixed, obtain liquid D;
5) liquid D is added drop-wise in 2% calcium chloride solution, formed spherical particle, immersion 2 hours to spherical particle into
Shape, takes out cleaning, and dries 3 hours at 60 DEG C, makes spherical particle dry forming, you can.
As further scheme of the invention:Step 1) in, the addition of the ethyl acetate is according to disposable foam
Depending on the addition of cutlery box, and the disposable foam cutlery box correspondence 4mL ethyl acetate of 1g.
As further scheme of the invention:Step 2) in, the preparation method of Suo Shu great Piao powder is:It is big by what is plucked
Piao is cleaned, and is dried at 80 DEG C, uses pulverizer attrition grinding, and crosses 50 mesh sieves, great Piao soaked in absolute ethyl alcohol 3h after sieving
Afterwards, cleaned with distilled water, then at 80 DEG C of drying, obtain powder, it is standby;The powder of above-mentioned drying is weighed, is used at 30 DEG C
The NaOH solution of 0.5mol/L is with solid-to-liquid ratio as 1:20 immersion 3h, immersion terminate after to distill water washing repeatedly until in neutrality,
Drying, obtains final product great Piao powder.
As further scheme of the invention:Step 3) in, the content of sodium alginate and polyvinyl alcohol in the liquid C
Respectively 1% and 5%.
Above-mentioned immobilized biological adsorbent can be used in adsorbing the heavy metal ion in water.
Compared with prior art, the invention has the beneficial effects as follows:
The present invention is prepared using disposable foam cutlery box, dried great Piao powder, sodium alginate and polyvinyl alcohol reagent
Solid particle, obtains immobilized biological adsorbent particle, and the particle has good absorption property and mechanical strength, with certain
Particle size, it is easy to filter or settle;With enough intensity, breaking deformation is difficult, recycled for multiple times has no that form becomes
Change;There is excellent absorption property to heavy metal ion in water;Particle is easy to operate at ambient pressure, controls, and carrier is readily formed;
It is the new way that exploiting natural resources of discarded object is utilized, advantage of lower cost.Absorbent particles prepared by the present invention be it is a kind of into
This is cheap, material source extensively, advantages of good adsorption effect, possess the new adsorbent for recycling performance, in heavy metal containing wastewater treatment
In have stronger using value.
Description of the drawings
Fig. 1 is three kinds of particles to Pb in water2+Absorption result figure.
Fig. 2 is PPB dosages to adsorbing Pb2+Impact figure.
Fig. 3 is that temperature adsorbs Pb to PPB2+Impact figure.
Fig. 4 is that adsorption time adsorbs Pb to PPB2+Impact figure.
Fig. 5 is Pb2+Initial concentration adsorbs Pb to PPB2+Impact figure.
Fig. 6 is that solution initial pH value adsorbs Pb to PPB2+Impact figure.
Fig. 7 is impact figure of the desorption to PPB absorption properties.
Specific embodiment
Technical scheme is described in more detail with reference to specific embodiment.
A kind of immobilized biological adsorbent of Adsorption of Heavy Metals, by disposable foam cutlery box, great Piao powder, sodium alginate and
Polyvinyl alcohol is made, and the mass ratio of the disposable foam cutlery box, great Piao powder, sodium alginate and polyvinyl alcohol is 4:4:1:
5。
The preparation method of Suo Shu great Piao powder is:Harvesting great Piao are cleaned, is dried at 80 DEG C, crushed with pulverizer and ground
Mill, and 50 mesh sieves are crossed, after great Piao are with soaked in absolute ethyl alcohol 3h after sieving, cleaned with distilled water, then at 80 DEG C of drying, obtain powder
Material, it is standby;The powder of above-mentioned drying is weighed, with the NaOH solution of 0.5mol/L with solid-to-liquid ratio as 1 at 30 DEG C:20 immersion 3h,
Immersion is multiple until in neutrality, drying, obtaining final product big Piao powder to distill water washing after terminating.In the present embodiment, it is preferred that in tide
Pluck the big Piao of wild life in Qiao Dongwoshi villages of state city.
The preparation method of the immobilized biological adsorbent of the Adsorption of Heavy Metals, step is as follows:
1) after disposable foam cutlery box is shredded, in being dissolved in ethyl acetate, liquid A is obtained, wherein, the ethyl acetate
Depending on addition of the addition according to disposable foam cutlery box, and the disposable foam cutlery box correspondence 4mL ethyl acetate of 1g;
2) great Piao powder is added into liquid A, after stirring, obtains liquid B;
3) by sodium alginate and polyvinyl alcohol, and heating for dissolving is in water, obtains liquid C;
4) liquid C is added into liquid B, and is uniformly mixed, obtain liquid D;
5) liquid D is added drop-wise in 2% calcium chloride solution, formed spherical particle, immersion 2 hours to spherical particle into
Shape, takes out cleaning, and dries 3 hours at 60 DEG C, makes spherical particle dry forming, you can.
Performance test
1st, medicine and instrument
Medicine:Sodium alginate used, PVAC polyvinylalcohol -124, NaOH, nitric acid, hydrochloric acid, absolute ethyl alcohol, anhydrous chlorine
Change calcium, ethyl acetate and be ommercially available AR.
Instrument:Accurate PH meters (PHS-3C, Shanghai You Ke instrument companies), atomic absorption spectrophotometer (AA/7000, day
This Shimadzu Corporation), digital display air dry oven (GZX-9146MBE, Shanghai Medical Equipment Plant of Bo Xun Industrial Co., Ltd.s), biochemical training
Foster case (LRH-150, the permanent Science and Technology Ltd. in Shanghai one), multiplex vavuum pump of circulating water type (SHD- III, Baoding high and new technology industrial development zone sunlight section
Religion instrument plant), pulverizer.
2nd, prepared by immobilization adsorbent
2.1st, prepared by blank bead
(1) mass ratio is taken for 5:1 polyvinyl alcohol and sodium alginate, heating for dissolving makes in the distilled water of certain volume
Its content is respectively 5% and 1%, is heated as thick liquid;
(2) thick liquid is added drop-wise in 2% calcium chloride solution, soaks 2 hours;Clean after immersion shaping, 50-60
3 hours are dried at DEG C to shaping, it is standby.Blank bead is designated as BLB.
2.2nd, prepared by great Piao powder immobilized spherule
(1) mass ratio is taken for 5:1 polyvinyl alcohol:Sodium alginate, heating for dissolving is in the water of certain volume so as to content
Respectively 5% and 1%, it is heated as thick liquid A;
(2) it is 4 accurately to weigh sodium alginate mass ratio in great Piao powder (great Piao powder and solution:1) it is added to above-mentioned glutinous
In thick liquid A, and it is well mixed, obtains thick liquid B, thick liquid B is added drop-wise in 2% calcium chloride solution, is formed little
Spherical particle, 2 hours of immersion take out cleaning to shaping, and 3 hours are dried at 60 DEG C to shaping, standby.Great Piao powder immobilizations
Particle is designated as PSB.
2.3rd, prepared by disposable foam cutlery box immobilized spherule
It is prepared using the preparation method of the embodiment of the present invention.The small spherical particles are designated as PPB.
3rd, adsorption test
3.1st, three kinds of beads are to Pb2+Absorption:Take the Pb (NO that concentration is 100mg/L3)2Solution 50mL, adds 250mL cones
In shape bottle, BLB, PSB and PPB pellets are respectively adopted and adsorb 2h in 25 DEG C, filter, determine Pb in filtrate2+And calculate absorption
Rate.
3.2nd, PPB dosages are to adsorbing Pb2+Impact:Take the Pb (NO that concentration is 100mg/L3)2Solution 50mL, adds respectively
Enter 0.5,1,1.5,2,2.5,3gPPB adsorb Pb in water in 25 DEG C2+, take out after 2h and filter, determine Pb in filtrate2+And calculate suction
Attached rate.
3.3rd, temperature adsorbs Pb to PPB2+Impact:Controlling reaction temperature is respectively 10 DEG C, 25 DEG C, 30 DEG C, 40 DEG C and 60
DEG C, weigh Pb in 1gPPB absorption water2+, remaining condition is same with 3.2, determines Pb in filtrate2+And calculate adsorption rate.
3.4th, adsorption time adsorbs Pb to PPB2+Impact:Controlling reaction temperature is 25 DEG C, adsorption time is respectively 0.5,
1st, 1.5,2,4,6,8,10h, remaining condition is same with 3.3.Determine Pb in filtrate2+And calculate adsorption rate.
3.5、Pb2+Initial concentration adsorbs Pb to PPB2+Impact:Solution initial p b2+Concentration is respectively 15,30,50,150,
200th, 300mg/L, thermostatic absorption reaction 2h, remaining condition is same with 3.4, determines Pb in filtrate2+And calculate adsorption rate.
3.6th, solution initial pH value adsorbs Pb to PPB2+Impact:Adjust solution ph and be respectively 2,3,4,5,6, in water
Pb2+Concentration is 50mg/L, and remaining condition is same with 3.1.Determine Pb in filtrate2+And calculate adsorption rate.
4th, circulation absorption test
(1) adsorption experiment:Take the Pb (NO that 50mL concentration is 100mg/L3)2Solution, control ph is 5, adds 1g PPB
Grain adsorbs 2h at 25 DEG C, filters, and determines Pb in filtrate2+And calculate adsorption rate.
(2) desorption experiment:Take and the PPB particles after adsorbing are completed in step (1), add and press in 1% hydrochloric acid solid-to-liquid ratio 1:
10 immersion 4h, with distillation water washing repeatedly to neutral, filter, dry for standby.
(3) adsorption experiment again:Weigh the Pb in the PPB granular absorption water in step (2) after 1g desorptions2+, remaining condition with
(1) it is same, filter, determine Pb in filtrate2+And calculate adsorption rate.
5th, adsorption test result
5.1st, BLB, PSB and PPB particle is to Pb2+Absorption
The result of experiment 3.1 is as shown in Figure 1.
As seen from Figure 1, BLB is to Pb in water2+There is certain adsorption capacity, this is because the sodium alginate contained in BLB
The heavy metal ion in water can be adsorbed.PSB and PPB are to Pb2+Adsorption rate is significantly larger than BLB, thus infers that addition great Piao powder has
Increase to effect the adsorption capacity of BLB.Disposable foam cutlery box is added to prepare PPB, the increase of particle mechanical strength, early stage in PSB
Observation shaping is preferable, even particle size, and oscillatory process is not broken in adsorption experiment, tests in follow-up repeatedly absorption-desorption
Middle grain shape is still remained intact.Because PPB has good absorption property and mechanical strength, below test and made using PPB
For adsorbent.
5.2nd, PPB dosages are to adsorbing Pb2+Impact
The result of experiment 3.2 is as shown in Figure 2.
As seen from Figure 2, in the Pb that 50mL concentration is 100mg/L2+In solution, when PPB dosages are less than 1.5g, with
The increase of dosage to Pb2+Adsorption rate increases rapidly;When dosage increases to 3.5g from 1.5g, continue to increase dosage pair
Adsorption rate affects less, and adsorption rate amplification tends towards stability.From ensureing adsorption effect, and cost-effective angle, subsequent experimental PPB
Dosage is 1g.
5.3rd, temperature adsorbs Pb to PPB2+Impact
The result of experiment 3.3 is as shown in Figure 3.
From the figure 3, it may be seen that in certain temperature range, the higher absorption of temperature is better, illustrates PPB to Pb2+Adsorption process may
It is the endothermic reaction.Under the conditions of due to 25 DEG C of room temperature, adsorption rate is up to more than 82%, it is contemplated that the situation of change of daily temperature, with
And to realize energy-saving and emission-reduction, it is proposed that adsorption reaction is controlled more than 25 DEG C.This experiment is carried out in Guangdong autumn, and room temperature is about
25 DEG C, therefore experiment is under room temperature and carries out.
5.4th, adsorption time adsorbs Pb to PPB2+Impact
The result of experiment 3.4 is as shown in Figure 4.
As shown in figure 4, with the prolongation of adsorption time, PPB is to Pb2+Absorption first rapid increase be presented then tend to flat
It is slow.When adsorption time is less than 2h, as time went on adsorption rate is rapidly increased to 82%;Then continue to extend adsorption time extremely
6h, adsorption rate increasess slowly, and only increases to 94% by 82%.Therefore, adsorption time is suitably controlled in 2h.
As shown in figure 4, reaction temperature is higher, the early stage rate of adsorption is faster.React 2h under the conditions of 10 DEG C and 25 DEG C respectively
Adsorption rate difference is 10.9%.But when the time 6h is extended to, adsorption rate gap is contracted to 0.8% under the conditions of two temperatures.It can be seen that,
Be conducive to improving adsorption rate by extending the reaction time.
5.5、Pb2+Initial concentration adsorbs Pb to PPB2+Impact
The result of experiment 3.5 is as shown in Figure 5.
As shown in Figure 5, as heavy metal initial concentration increases, PPB is to Pb2+Adsorption rate is presented downward trend, and temperature
Higher, adsorption rate increases with concentration and fall is bigger.When temperature is 40 DEG C, Pb2+Initial concentration 15mg/L is increased to
300mg/L, then adsorption rate decline 29.9%.Therefore, PPB is properly applied to the adsorption treatment of low concentration heavy metal water.
5.6th, solution initial pH value adsorbs Pb to PPB2+Impact
The result of experiment 3.6 is as shown in Figure 6.
It will be appreciated from fig. 6 that when solution initial pH value≤4, adsorption rate is 67%~70%.When solution initial pH value is increased to
When 5, adsorption rate increases to rapidly 84.3%.Solution initial pH value affects PPB to Pb2+Absorption property, pH value control more than 5
Most preferably.
6th, circulation absorption result of the test
The result of experiment 4 is as shown in Figure 7.
As shown in Figure 7, by absorption-desorption-adsorb again, PPB is to Pb2+The 2nd adsorption rate than the 1st time decline 13 hundred
Branch, it is seen that Pb2+Combined with PPB relatively closely, be difficult desorption.But the 2nd absorption-desorption-adsorb again, PPB is to Pb2+Absorption
Rate declines not substantially, and the 3rd time adsorption rate only declines 2.6% than the 2nd time.It is considered that PPB particles are through multiple circulation absorption-solution
Suction still keeps certain adsorption capacity, can inquire into follow-up research and its desorption effect how is improved under the conditions of optimal desorption
Rate, to strengthen recycling efficiency.
7th, conclusion (of pressure testing)
The present invention adopts disposable foam cutlery box, dried great Piao plant powders, sodium alginate and polyvinyl alcohol reagent
Prepare solid particle, the immobilized biological adsorbent particle of acquisition, the particle has good absorption property and a mechanical strength, 60
6h adsorption rates are reacted under the conditions of DEG C up to 100%.Through 3 absorption-desorptions-adsorb again, grain shape keeps complete, and adsorbs
Rate is still more than 68%.PPB be a kind of with low cost, material source extensively, advantages of good adsorption effect, possess and recycle the new of performance
Type adsorbent, has stronger using value in heavy metal containing wastewater treatment.
The better embodiment of the present invention is explained in detail above, but the present invention is not limited to above-mentioned embodiment party
Formula, in the ken that one skilled in the relevant art possesses, can be with the premise of without departing from present inventive concept
Various changes can be made.
Claims (8)
1. a kind of immobilized biological adsorbent of Adsorption of Heavy Metals, it is characterised in that by disposable foam cutlery box, great Piao powder,
Sodium alginate and polyvinyl alcohol are made.
2. the immobilized biological adsorbent of Adsorption of Heavy Metals according to claim 1 a, it is characterised in that sex vesicle
The mass ratio of foam cutlery box, great Piao powder, sodium alginate and polyvinyl alcohol is 4:4:1:5.
3. the immobilized biological adsorbent of Adsorption of Heavy Metals according to claim 2, it is characterised in that the sodium alginate
AR is with polyvinyl alcohol.
4. a kind of preparation method of the immobilized biological adsorbent of the Adsorption of Heavy Metals as described in claim 1-3 is arbitrary, it is special
Levy and be, step is as follows:
1) after disposable foam cutlery box is shredded, in being dissolved in ethyl acetate, liquid A is obtained;
2) great Piao powder is added into liquid A, after stirring, obtains liquid B;
3) by sodium alginate and polyvinyl alcohol, and heating for dissolving is in water, obtains liquid C;
4) liquid C is added into liquid B, and is uniformly mixed, obtain liquid D;
5) liquid D is added drop-wise in 2% calcium chloride solution, forms spherical particle, immersion takes for 2 hours to spherical particle shaping
Go out cleaning, and dry 3 hours at 60 DEG C, make spherical particle dry forming, you can.
5. the preparation method of the immobilized biological adsorbent of Adsorption of Heavy Metals according to claim 4, it is characterised in that step
It is rapid 1) in, depending on the addition of the addition of the ethyl acetate according to disposable foam cutlery box, and the disposable foam cutlery boxs of 1g
Correspondence 4mL ethyl acetate.
6. the preparation method of the immobilized biological adsorbent of Adsorption of Heavy Metals according to claim 4, it is characterised in that step
It is rapid 3) in, the content of sodium alginate and polyvinyl alcohol is respectively 1% and 5% in the liquid C.
7. the preparation method of the immobilized biological adsorbent of Adsorption of Heavy Metals according to claim 4, it is characterised in that step
It is rapid 2) in, the preparation method of Suo Shu great Piao powder is:Harvesting great Piao are cleaned, is dried at 80 DEG C, crushed with pulverizer and ground
Mill, and 50 mesh sieves are crossed, after great Piao are with soaked in absolute ethyl alcohol 3h after sieving, cleaned with distilled water, then at 80 DEG C of drying, obtain powder
Material, it is standby;The powder of above-mentioned drying is weighed, with the NaOH solution of 0.5mol/L with solid-to-liquid ratio as 1 at 30 DEG C:20 immersion 3h,
Immersion is multiple until in neutrality, drying, obtaining final product big Piao powder to distill water washing after terminating.
8. purposes of the immobilized biological adsorbent as described in claim 1-3 is arbitrary in Adsorption of Heavy Metal Ions.
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CN108905999A (en) * | 2018-07-20 | 2018-11-30 | 武汉沃特工程技术有限公司 | A kind of new bio charcoal plural gel and its preparation method and application |
CN111701566A (en) * | 2020-06-30 | 2020-09-25 | 广东工业大学 | Adsorbent and preparation method and application thereof |
CN115386136A (en) * | 2022-08-30 | 2022-11-25 | 南京大学 | Preparation method and application of aminated polyacrylamide foam adsorbent |
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