CN101601991A - Remove biomass adsorbent and preparation, application and the renovation process of lead ion in the waste water - Google Patents
Remove biomass adsorbent and preparation, application and the renovation process of lead ion in the waste water Download PDFInfo
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- CN101601991A CN101601991A CNA200910043760XA CN200910043760A CN101601991A CN 101601991 A CN101601991 A CN 101601991A CN A200910043760X A CNA200910043760X A CN A200910043760XA CN 200910043760 A CN200910043760 A CN 200910043760A CN 101601991 A CN101601991 A CN 101601991A
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Abstract
The invention discloses a kind of biomass adsorbent and preparation, application and renovation process of removing lead ion in the waste water, this biomass adsorbent is graininess, it is to be carrier with calcium alginate and gelatin, be embedded with the shaddock ped powder in the carrier, the mass ratio of calcium alginate, gelatin and shaddock ped powder is (8～10): (4～5): 1, this biomass adsorbent is to obtain adsorbent embedding body with the mixed glue solution of sodium alginate and gelatin parcel shaddock ped powder, splashes into CaCl then
2Solidify in the solution, use deionized water rinsing again, and after freeze drying, prepare.Adding biomass adsorbent of the present invention in waste water, is that adsorption treatment is not shorter than 30min under 3.5～7.0 the normal temperature in the pH value, can remove the lead ion in the waste water substantially.Biomass adsorbent of the present invention has that raw material sources are abundant, cost is low, mechanical strength is high, to the advantages such as advantages of good adsorption effect of lead ion in the waste water.
Description
Technical field
The present invention relates to the processing of waste water or sewage, relate in particular to a kind of biomass adsorbent and preparation thereof, also relate to the method for utilizing this biomass adsorbent to remove heavy metal in waste water and the renovation process of biomass adsorbent.
Background technology
Along with improving constantly of science and technology development and human living standard, a large amount of pollutants enters water environment by different approach, causes aquatic ecological environmental quality severe exacerbation, and wherein the pollution of heavy metal is particularly serious.And the lead in the heavy metal is a kind of serious environmental poison and neural poison, to all toxic effects of system such as the nerve of human body, blood, digestion, uropoiesis, reproduction, immunity, and plumbous toxicity has chronicity and persistence, it is administered caused the great attention and the concern of international community.
Traditional lead removal method mainly contains chemical precipitation method, electrolysis, ion-exchange, membrane processing method and mixed processing method thereof etc., but there are defectives such as complex process, complex operation, operating cost height, generation secondary pollution in these methods when handling the low concentration lead waste water, press for a kind of technology of simple and effective processing lead waste water.Adopt new and effective cheap biomass adsorbent (as agricultural wastes) to handle heavy metal, can reduce processing cost, can make full use of existing green resource again, beginning more and more comes into one's own, but how it is effectively applied to the processing of lead ion in the waste water, just becomes those skilled in the art's technical issues that need to address.
Summary of the invention
The technical problem to be solved in the present invention is to overcome the deficiencies in the prior art, provide that a kind of raw material sources are abundant, with low cost, mechanical strength is high, the biomass adsorbent of lead ion in the removal waste water of advantages of good adsorption effect, also at this biomass adsorbent provide easy to operate, equipment simple, reaction temperature and, weak point consuming time, this adsorbent preparation method that efficient is high, the method for sorbent treatment lead waste water and the method for adsorbent reactivation.
For solving the problems of the technologies described above, the technical scheme that the present invention proposes is a kind of biomass adsorbent of removing lead ion in the waste water, it is characterized in that: described biomass adsorbent is graininess, it is to be carrier (this mixed carrier is similar to the skeleton backing material) with calcium alginate and gelatin, be embedded with shaddock ped powder (the shaddock ped powder is filled in the middle of the carrier material) in the described carrier, the mass ratio of described calcium alginate, gelatin and shaddock ped powder is (8～10): (4～5): 1.The particle diameter of described biomass adsorbent is preferably 2～4mm, and described shaddock ped powder was preferably the shaddock ped powder behind 50 mesh sieves.
The present invention also provides a kind of preparation method who removes the biomass adsorbent of lead ion in the waste water, may further comprise the steps: the mixed glue solution parcel shaddock ped powder with sodium alginate and gelatin obtains adsorbent embedding body, then described adsorbent embedding body is splashed into CaCl
2Solidify in the solution and make elementary adsorbent; Wash described elementary adsorbent repeatedly with deionized water again, after obtain described biomass adsorbent after the freeze drying.In this preparation method, the shaddock ped powder of using is preferably crossed the shaddock ped powder behind 50 mesh sieves, employing be immobilization embedded mode, this embedding mode is simple to operate, and is less to the influence of shaddock ped cytoactive.The biomass adsorbent for preparing at last with this shaddock ped powder is regular graininess, and its particle diameter generally is distributed in the scope of 2～4mm, has advantages such as particle diameter is little and even, specific area big, advantages of good adsorption effect, is suitable for the processing of low concentration lead waste water.
Among the above-mentioned preparation method, the consumption of described shaddock ped powder is preferably every 100ml mixed glue solution and uses shaddock ped powder 3～5g.
Among the above-mentioned preparation method, the described temperature that is used to wrap up the mixed glue solution of shaddock ped powder preferably is controlled at 60 ℃～80 ℃; Be used to solidify the CaCl of described adsorbent embedding body
2The temperature of solution is preferably-1 ℃～-4 ℃, at described CaCl
2The time that is cured in the solution preferably is controlled at 1～6h.
Among the above-mentioned preparation method, the temperature during described freeze drying preferably is controlled at-20 ℃～-40 ℃, and the cryodesiccated time is preferably 12～20h.
Among the above-mentioned preparation method, the mass concentration of the sodium alginate that contains in the described mixed glue solution is preferably 3%～6%, and the mass concentration of the gelatin that contains in the described mixed glue solution is preferably 2%～5%; Described CaCl
2The mass concentration of solution is preferably 2%～6%.
The living beings sorbing material shaddock ped that adopts in the technique scheme is abundant in the output of China south provinces and cities, and cheap, its absorption property excellence is a kind of environment-friendly type heavy metal biological sorbing material with broad prospect of application.The shaddock ped main component is lignin, cellulose, hemicellulose and most pectic substance, contain a large amount of carboxyls in the polygalacturonic acid of pectic substance, possesses stronger metal ion binding ability, but shortcomings such as its mechanical strength is little, perishable bring very big inconvenience for the adsorption operations of shaddock ped, therefore shaddock ped need be carried out immobilization and handle and improve its mechanical performance.The fixation support material sodium alginate that adopts in the technique scheme is a kind of natural macromolecular material, good biocompatibility is arranged, to biological nontoxic, mass-transfer performance is good, and can not produce secondary pollution, the biomass adsorbent mechanical strength height that makes is a kind of good adsorbing agent carrier material.The another kind of fixation support material gelatin that adopts in the technique scheme dissolves in hot water (50 ℃～80 ℃), forms the thermal reversibility gel, has the effect of suction and support frame, after water-soluble, can attract each other, interweave, form the network structure of folded lamination layer, and condense with temperature decline, the shaddock ped powder is filled fully in the gel space, can keep stable form, bear bigger load, reduce fragility, help the adsorbent moulding, and indeformable.
On the basis of technique scheme, the present invention also provides the described biomass adsorbent of a kind of usefulness to remove the method for lead ion in the waste water, the steps include: in pending waste water, to add described biomass adsorbent, carry out adsorption treatment under be 3.5～7.0 in the pH value normal temperature condition of (generally regulating) by adding NaOH solution or hydrochloric acid, the time of controlling described adsorption treatment is not shorter than 30min, the basic lead ion of removing in the waste water after adsorption treatment is finished, its adsorption rate reaches as high as 99.5%, and is minimum also near 70%.
In the above-mentioned removal waste water in the method for lead ion, through experiment repeatedly to test when, each optimal process parameter controlled condition is: the initial concentration of lead ion preferably is controlled at 50～200mgL in the described pending waste water
-1(most preferably be 110mgL
-1); The addition of biomass adsorbent preferably is controlled at 0.1～0.5gL in the described waste water
-1(most preferably be 0.3gL
-1); PH value in the described adsorption treatment process preferably is controlled at 4.5～6.5 (most preferably being 5.5); The time of described adsorption treatment preferably is controlled at 1～10h (most preferably being 4h).Through above-mentioned every parameters Optimization is controlled and is handled, the adsorption rate of lead ion can be basicly stable more than 90% or near 90% in the waste water, the biomass adsorbent of finishing after the adsorption process can separate from wastewater treatment system at an easy rate, through reclaim, reusable after the regeneration.
Supporting as to above-mentioned lead waste water processing method, the present invention also provides a kind of renovation process of described biomass adsorbent, the steps include: to finish the described biomass adsorbent recovery of lead ion adsorption process in the waste water, biomass adsorbent after will reclaiming then joins and carries out wash-out in the citric acid, the quality of the biomass adsorbent of every liter of citric acid wash-out is 10～30g, the time of wash-out is 15～25min, obtains the biomass adsorbent of regenerating again after centrifugation.
In the above-mentioned renovation process, the concentration of described citric acid is preferably 100～200mmolL
-1(optimum is 100mmolL
-1); The rotating speed of described centrifugation is preferably 4000～8000rmin
-1(optimum is 4500rmin
-1); The time of described centrifugation is preferably 10～20min (the optimum 15min of being).
Compared with prior art, the invention has the advantages that: at first, a kind of advantages of good adsorption effect, abundant, the with low cost biological sorbing material of raw material sources have been selected, and two kinds of adsorbing agent carrier materials with strong complementarity, that performance good, cost is low have been selected at this biology sorbing material, utilize investment (method for immobilizing cell) that biological sorbing material is fixed then, the living beings cell is locked in the specific macromolecule network structure.This structure is closely to being enough to prevent the cell seepage, but can allow substrate infiltration and product to spread, and the pair cell activity influence is less, the intensity of the immobilized cell of making is higher, improved greatly should the biology sorbing material mechanical performance and mechanical strength.The biomass adsorbent of the present invention's preparation can carry out large-scale production and application more easily, and scale detects and remove the heavy metal lead ion in the waste water.That the preparation method of biomass adsorbent of the present invention, method of wastewater treatment and renovation process all have is easy to operate, equipment simple, reaction temperature and, advantage such as weak point consuming time, allow rapid loading and simple and efficient wash-out, greatly improved production efficiency.
The specific embodiment
Embodiment 1
A kind of biomass adsorbent of the present invention specifically prepares by following steps:
1, the processing of shaddock ped powder: remove outermost bluish yellow color table skin after discarded shaddock skin cleaned with clear water, be cut into 1cm after air-dry under the room temperature
2The fragment of size, with its with distilled water clean several all over after air-dry under room temperature again; Then at 65 ℃ of following baking 48h, make the following shaddock ped powder of particle diameter 600 μ m after crossing 50 mesh sieves, place in the drier stand-by;
2, solution preparation: with CaCl
2Be dissolved in the deionized water, make mass concentration through stirring and be 6% CaCl
2Solution (being embedding treatment liquid); Sodium alginate and gelatin are put into deionized water, are to stir under 80 ℃ of conditions to make the mixed glue solution of sodium alginate and gelatin in temperature, and wherein the mass concentration of sodium alginate is 5%, and the mass concentration of gelatin is 3%;
3, the preparation of embedding body: the shaddock ped powder that makes in the step 1 is added in the mixed glue solution of 80 ℃ sodium alginate making in the step 2 and gelatin, the consumption of shaddock ped powder is to add 3g in every 100ml mixed glue solution, makes adsorbent embedding body after mixing;
4, curing molding: the adsorbent embedding body that makes in the step 3 is added in-1 ℃ the embedding treatment liquid of preparation in the step 2, behind the curing 6h, obtain elementary biological adsorption agent after filtration; Use deionized water rinsing then 2～5 times, behind freeze drying 20h under-40 ℃ of conditions, make the biomass adsorbent that particle diameter is 2～4mm.
The biomass adsorbent that method for preparing obtains is graininess, and it is to be carrier with calcium alginate and gelatin, is embedded with the shaddock ped powder in the carrier, and wherein the mass ratio of calcium alginate, gelatin and shaddock ped powder is 9.2: 4.6: 1.
The biomass adsorbent for preparing with embodiment 1 carries out the removal Pb in following examples 2～5
2+Adsorption test.
Embodiment 2
Get 50mL Pb
2+Concentration is 100mgL
-1Lead waste water, place the 250mL conical flask, regulate this and contain Pb
2+The pH value of waste water changes in 1～7 scope, under different pH value conditions, all adds the biomass adsorbent of 0.015g and in 30 ℃ of constant temperature shaking tables vibration 4h (oscillation rate 150rmin at every turn
-1); Adsorption treatment is taken a sample after finishing, and sample is through 4500rmin
-1Centrifugal 10min, lower floor are the biomass adsorbent that has adsorbed lead ion.With the Pb in the 3510 atomic absorption spectrophotometer supernatants
2+Concentration, measurement result is as shown in table 1:
Table 1: biomass adsorbent under different pH condition to Pb
2+Removal effect
| The pH value | 1.8 | 2.5 | 3.5 | 4.5 | 5.5 | 6.5 |
| Adsorption rate (%) | 18.4 | 326 | 68.5 | 99.0 | 99.2 | 98.8 |
Pb
2+Adsorption rate calculate (down with) according to following formula:
In the following formula, R is an adsorption rate, C
0Be Pb in the waste water before adsorbing
2+Concentration (mgL
-1), C is the Pb in the waste water of absorption back
2+Concentration (mgL
-1).
By last table 1 as can be known, this biomass adsorbent is under 5.5 the condition in the pH value, and it is best that adsorption effect reaches.
Embodiment 3
Respectively get 50mL Pb
2+Initial concentration is 50mgL
-1, 70mgL
-1, 90mgL
-1, 110mgL
-1, 130mgL
-1, 150mgL
-1, 200mgL
-1Contain Pb
2+Waste water places the 250mL conical flask respectively, and the pH value of regulating waste water is 5.5, respectively to wherein adding the 0.015g biomass adsorbent, constant temperature shaking table vibration 4h (oscillation rate 150rmin under 30 ℃ of temperature
-1).Adsorption treatment is taken a sample after finishing, and sample is through 4500rmin
-1Centrifugal 10min, lower floor are and have adsorbed Pb
2+Biomass adsorbent.With the Pb in the 3510 atomic absorption spectrophotometer supernatants
2+Concentration, the result is as shown in table 2 below:
Table 2: biomass adsorbent is at the Pb that contains of different initial concentrations
2+In the waste water to Pb
2+Removal effect
| Initial p b 2+Concentration (mgL -1) | 50 | 70 | 90 | 110 | 130 | 150 | 200 |
| Adsorption rate (%) | 99.5 | 99.4 | 99.2 | 99.1 | 98.0 | 90.5 | 85.2 |
By last table 2 as can be known, to initial concentration less than 110mgL
-1Contain Pb
2+The adsorption rate of waste water all is higher than 99%, and concentration is 110mgL
-1Contain Pb
2+Waste water absorption back Pb
2+Residual volume be 0.9mgL
-1, reach highest standard (total Pb of the highest permission concentration of emission of first kind pollutant
2+＜10mgL
-1).Therefore, biomass adsorbent of the present invention for concentration of treatment less than 110mgL
-1Contain Pb
2+The waste water effect is remarkable.
Embodiment 4
Get 5 groups of 50mL Pb
2+Initial concentration is 110mgL
-1Contain Pb
2+Waste water contains Pb to these 5 groups
2+Add the biomass adsorbent of 0.005g, 0.01g, 0.015g, 0.02g, 0.025g in the waste water respectively, the pH value of regulating waste water then is 5.5,30 ℃ of constant temperature shaking table vibration 4h (oscillation rate 150rmin
-1).Adsorption treatment is taken a sample after finishing, and sample is through 4500rmin
-1Centrifugal 10min, lower floor are and have adsorbed Pb
2+Biomass adsorbent.With the Pb in the 3510 atomic absorption spectrophotometer supernatants
2+Concentration, the result is as shown in table 3 below:
Table 3: biomass adsorbent under the different amounts condition to Pb
2+Removal effect
| Adsorbent consumption (gL -1) | 0.1 | 0.2 | 0.3 | 0.4 | 0.5 |
| Adsorption rate (%) | 87.5 | 95.6 | 99.2 | 99.0 | 98.5 |
As shown in Table 3, when the biomass adsorbent consumption be 0.3gL
-1The time, Pb
2+Removal effect best, and cost is less relatively.
Embodiment 5
Get 7 groups of 50mL Pb
2+Initial concentration is 110mgL
-1Contain Pb
2+Waste water is regulated the pH value and is 5.5, all adds biomass adsorbent 0.015g in every group of waste water, 30 ℃ of constant temperature shaking table (oscillation rate 150rmin
-1) under carry out adsorption test, each the group adsorption treatment time be respectively 10min, 30min, 60min, 120min, 240min, 360min and 600min.Adsorption treatment is taken a sample after finishing, and sample is through 4500rmin
-1Centrifugal 10min, lower floor are and have adsorbed Pb
2+Biomass adsorbent.With the Pb in the 3510 atomic absorption spectrophotometer supernatants
2+Concentration, the result is as shown in table 4 below:
Table 4: biomass adsorbent under different adsorption time conditions to Pb
2+Removal effect
| Adsorption time (min) | 10 | 30 | 60 | 120 | 240 | 360 | 600 |
| Adsorption rate (%) | 62.3 | 73.5 | 90.2 | 94.6 | 99.3 | 99.2 | 98.5 |
As shown in Table 4, after adsorption time surpassed 4h, adsorption rate did not improve, along with the suction phenomenon generation is separated in the prolongation of adsorption time in addition, so the Best Times of adsorption reaction is 4h.
Embodiment 6
Fetch lead waste water 1m from certain storage battery factory
3, record its Pb
2+Concentration is 65.7mgL
-1, regulating the pH value is 5～6, to wherein adding biomass adsorbent 0.3kg, and 30 ℃ of temperature, oscillation rate 150rmin
-1Condition under the absorption of vibrating, directly filter separating adsorbent behind the 4h.With the Pb in the waste water after the filtration of 3510 atomic absorption spectrophotometers
2+Concentration, lead waste water clearance are 99.2%.
Embodiment 7
To finish Pb among the embodiment 2～6
2+The biomass adsorbent of adsorption process is used 100mmo1L after reclaiming
-1Citric acid the biomass adsorbent after reclaiming is soaked wash-out, the time of soaking wash-out is 20min, again at 4500rmin
-1Rotating speed under centrifugal 15min, the biomass adsorbent that obtains regenerating.
Claims (10)
1, a kind of biomass adsorbent of removing lead ion in the waste water, it is characterized in that: described biomass adsorbent is graininess, it is to be carrier with calcium alginate and gelatin, be embedded with the shaddock ped powder in the described carrier, the mass ratio of described calcium alginate, gelatin and shaddock ped powder is (8～10): (4～5): 1.
2, biomass adsorbent according to claim 1 is characterized in that: the particle diameter of described biomass adsorbent is 2～4mm, and described shaddock ped powder was the shaddock ped powder behind 50 mesh sieves.
3, a kind of preparation method who removes the biomass adsorbent of lead ion in the waste water may further comprise the steps: the mixed glue solution parcel shaddock ped powder with sodium alginate and gelatin obtains adsorbent embedding body, then described adsorbent embedding body is splashed into CaCl
2Solidify in the solution and make elementary adsorbent; Wash described elementary adsorbent repeatedly with deionized water again, after obtain described biomass adsorbent after the freeze drying.
4, preparation method according to claim 3 is characterized in that: the consumption of described shaddock ped powder is that every 100ml mixed glue solution uses shaddock ped powder 3～5g.
5, according to claim 3 or 4 described preparation methods, it is characterized in that: the described temperature that is used to wrap up the mixed glue solution of shaddock ped powder is 60 ℃～80 ℃; Be used to solidify the CaCl of described adsorbent embedding body
2The temperature of solution is-1 ℃～-4 ℃, at described CaCl
2The time that is cured in the solution is controlled at 1～6h; Temperature during described freeze drying is-20 ℃～-40 ℃, and the cryodesiccated time is 12～20h.
6, according to claim 3 or 4 described preparation methods, it is characterized in that: the mass concentration of the sodium alginate that contains in the described mixed glue solution is 3%～6%, and the mass concentration of the gelatin that contains in the described mixed glue solution is 2%～5%; Described CaCl
2The mass concentration of solution is 2%～6%; Described shaddock ped powder was the shaddock ped powder behind 50 mesh sieves.
7, a kind of biomass adsorbent that each preparation method makes in the described or claim 3～6 with claim 1 or 2 is removed the method for lead ion in the waste water, the steps include: in pending waste water, to add described biomass adsorbent, be to carry out adsorption treatment under 3.5～7.0 the normal temperature condition in the pH value, the time of controlling described adsorption treatment is not shorter than 30min, the basic lead ion of removing in the waste water after adsorption treatment is finished.
8, method according to claim 7 is characterized in that: the initial concentration of lead ion is controlled at 50～200mgL in the described pending waste water
-1The addition of biomass adsorbent is controlled at 0.1～0.5gL in the described pending waste water
-1PH value in the described adsorption treatment process is controlled at 4.5～6.5; The time of described adsorption treatment is controlled at 1～10h.
9, a kind of renovation process of the biomass adsorbent that each preparation method makes in the described or claim 3～6 with claim 1 or 2, the steps include: to finish the recovery of the biomass adsorbent after the lead ion adsorption treatment in the waste water, biomass adsorbent after will reclaiming then joins and carries out wash-out in the citric acid, the quality of the biomass adsorbent of every liter of citric acid wash-out is 10～30g, the time of wash-out is 15～25min, obtains the biomass adsorbent of regenerating again after centrifugation.
10, renovation process according to claim 9 is characterized in that: the concentration of described citric acid is 100～200mmolL
-1The rotating speed of described centrifugation is 4000～8000rmin
-1, the time of described centrifugation is 10～20min.
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|---|---|---|---|
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| CN116099509A (en) * | 2023-01-13 | 2023-05-12 | 安徽工业大学 | Sodium alginate/gelatin biochar multi-element composite material, preparation method and method for treating cadmium in water body |
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Open date: 20091216 |