CN105289560A - Chitosan-based composite adsorbent capable of synergistically and efficiently removing positive and negative ions of heavy metals and preparation method thereof - Google Patents
Chitosan-based composite adsorbent capable of synergistically and efficiently removing positive and negative ions of heavy metals and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a chitosan-based composite adsorbent capable of synergistically and efficiently removing positive and negative ions of heavy metals and a preparation method thereof and belongs to the technical field of heavy metal wastewater treatment. The preparation method of the chitosan-based composite adsorbent comprises the steps that A, chitosan powder is dissolved in an acetic acid solution to form a chitosan mother solution, ferric sulfate and polyethyleneimine are put into the chitosan mother solution, uniform stirring is performed, and a mixed mother solution is obtained after preliminary crosslinking is performed by using epoxy chloropropane; B, the mixed mother solution is pumped into a coagulating bath, and composite microspheres are obtained through precipitation solidification; C, the composite microspheres are taken out and put into asodium hydroxide water solution, crosslinking is performed by using epoxy chloropropane to obtain crosslinked microspheres, and the crosslinked microspheres are washed by using distilled water till the crosslinked microspheres are neutral and then are dehydrated and saved for standby application. The chitosan-based composite adsorbent is simple in preparation, low in cost, stable in structure, superior in performance, can synergistically and efficiently remove the positive and negative ions of heavy metals and has wide application prospect on the aspect of synergistic control of combined pollutants of heavy metal positive and negative ions.
Description
Technical field
The invention belongs to technical field of heavy metal wastewater treatment, more particularly, relate to and a kind ofly work in coordination with chitosan-based compound adsorbent of efficient removal heavy metal zwitterion and preparation method thereof.
Background technology
The poisoning harmful heavy metals anion of industrial wastewater, surface water and underground water is (as chromate, arsenate) and cation (as copper ion, cadmium ion, lead ion) often mixing coexist, all water quality safety and environmental health are constituted a serious threat.Common heavy metal pollution of water body is cut down technology and is comprised chemical precipitation method, absorption method, bio-flocculation process and membrane separation process etc.Absorption method wherein based on high-efficiency adsorbent becomes selection process because of advantages such as easy and simple to handle, high efficient and reliable, renewable and recyclings.
Common adsorbents and simple function base adsorbent can only form effective absorption to the one in metal cation or anion, therefore need used in combination for various conventional adsorbent or plural serial stage to be used to be formed zwitterion to remove effectively altogether, this can increase Operating Complexity and investment operating cost undoubtedly greatly.
Amphiphilic adsorbent, because possessing two kinds or more function bases simultaneously, can work in coordination with trapping negative and positive heavy metal ion, so become investigation and application focus.The synthesis of tradition Amphoteric Materials is divided into two steps usually, namely on parent, Cation adsorption function base is first modified, introduce Anion-adsorption function base again, or first modify Anion-adsorption function base, introduce Cation adsorption function base again, if application number is 201010207804.0, Shen Qing Publication day is preparation method and the application that the patent document on October 20th, 2010 discloses a kind of amphoteric chelate sorbent containing agricultural straw, adopt agricultural stalk and epoxychloropropane, chloroacetic acid is raw material, using trimethylamine or triethylamine as graft reaction agent, with ethylenediamine, diethylenetriamine or triethylene tetramine are prepared from as crosslinking agent, application number is 201210110877.7, Shen Qing Publication day is stalk and the method for making thereof that the patent document of on 08 08th, 2012 discloses that a kind of modification becomes amphoteric adsorbent, it is by stalk and the reaction of 3-chloro-2-hydroxypropyl-trimethyl ammonium chloride in alkaline solution, the cellulose or lignin molecule chain of stalk are grafted with the stalk of 2-hydroxypropyl-trimethyl ammonium chloride, then, again in ethanol-water mixed solvent with chloroacetate reaction, grafting aceticoceptor on stalk, forms the stalk that modification becomes anion and cationic amphoteric adsorbent, document Chromate (CrO
4 2-) andcopper (Cu
2+) adsorptionbydual-functionalionexchangeresinsmadefromagri culturalby-products, WaterResearch40 (2006) 2541 – 2548.The method preparing amphiphilic adsorbent disclosed in above patent or document is due to can be limited and limit the zwitterion adsorption function radix amount successively introduced for the avtive spot modified on parent, cause the adsorption capacity of heavy metal zwitterion all not enough, and preparation method need carry out in two steps, complicated operation, cost is higher.
Hydrous iron oxide particle, because of containing enriching surface hydroxyl, has good adsorption properties to anionic metal, and its raw material sources are extensive in addition, cheap, by regulating pH realize its regeneration and reuse, thus becomes desirable anion adsorbent.But hydrous iron oxide particle size is minimum, directly can produces larger resistance or cause separation difficulty during application, causing adsorption system cannot stable operation.By hydrous iron oxide particle load or to be embedded in polymer matrix be solve the effective way of its through engineering approaches application bottleneck, as chitosan imbedded (AnjaliGuptaet.al, Preparationandevaluationofiron-chitosancompositesforremo valofAs (III) andAs (V) fromarseniccontaminatedreallifegroundwater, waterresearch43 (2009) 3862 – 3870).But the easy drop of embedding shell glycan prepared by conventional method goes out iron ion, cause secondary pollution and adsorption capacity loss, and it is not high to the adsorption capacity of metal cation, need further in addition modification.
Summary of the invention
1. the problem that will solve
Complicated process of preparation is there is for existing amphiphilic adsorbent, adsorption capacity is low, the deficiencies such as easy generation secondary pollution, the invention provides and a kind ofly work in coordination with chitosan-based compound adsorbent of efficient removal heavy metal zwitterion and preparation method thereof, inorganic hydrated ferric oxide is embedded in chitosan basal body and prepares complex carrier, and further for the easy stripping of iron ion in chitosan base composite absorbent, and the problem that heavy metal Cation adsorption capacity is little, polymine is added in composite adsorption, prepare a kind of stable performance and the chitosan-based compound adsorbent of efficient removal heavy metal zwitterion can be worked in coordination with.
2. technical scheme
In order to solve the problem, the technical solution adopted in the present invention is as follows:
Work in coordination with a preparation method for the chitosan-based compound adsorbent of efficient removal heavy metal zwitterion, the steps include:
A) Chitosan powder be dissolved in acetic acid solution form shitosan mother liquor, in shitosan mother liquor, add ferric sulfate and polymine, stir, and just crosslinked with epoxychloropropane after obtain mixing mother liquor;
B) gained mixing mother liquor is added in coagulating bath, solidify through precipitation and obtain complex microsphere;
C) take out complex microsphere, be added in the aqueous solution of NaOH, carry out rear crosslinked with epoxychloropropane, obtained crosslinked microsphere, be washed till neutrality with distilled water, dehydrated preservation is for subsequent use.
Preferably, steps A) in shitosan mother liquor in, the mass concentration of shitosan is 2 ~ 50g/L, and the volumetric concentration of acetic acid is 1 ~ 8%, and solution temperature is 20 ~ 80 DEG C, and dissolution time is 2 ~ 10h.
Preferably, steps A) in the ferric sulfate that adds in shitosan mother liquor and polymine, make sulfuric acid iron speciation in mixing mother liquor be 5 ~ 60g/L, the mass concentration of polymine is 10 ~ 100g/L.
Preferably, steps A) in mixing mother liquor the volumetric concentration of crosslinking agent epoxychloropropane be 0.5 ~ 4%, crosslinking temperature is 20 ~ 80 DEG C, and crosslinking time is 2 ~ 20h.
Preferably, step B) in coagulating bath used be the mixed solution being dissolved with in sodium sulphate, NaOH, sodium phosphate trimer and sodium pyrophosphate one or more.
Preferably, step B) in coagulating bath used be the mixed aqueous solution that the mass concentration of NaOH and sodium sulphate is respectively 10 ~ 200g/L and 20 ~ 200g/L.
Preferably, described step C) in complex microsphere dosage be 2 ~ 40g/L, the pH of sodium hydrate aqueous solution is 10 ~ 14.
Preferably, described step C) reaction system in the volumetric concentration of epoxychloropropane be 0.01 ~ 0.5%, crosslinking temperature is 20 ~ 80 DEG C, and crosslinking time is 2 ~ 20h.
The chitosan-based compound adsorbent that above-mentioned a kind of preparation method working in coordination with the chitosan-based compound adsorbent of efficient removal heavy metal zwitterion prepares.
3. beneficial effect
Compared to prior art, beneficial effect of the present invention is:
(1) the invention provides a kind of simple effective method preparing organo-mineral complexing adsorbent, overcome conventional amphiphilic adsorbent complicated process of preparation, the shortcoming little to metal zwitterion adsorption capacity, and by being embedded in by hydrous iron oxide particle in cheap shitosan parent, efficiently solve a difficult problem for mineral particulates through engineering approaches application;
(2) in the present invention, biological polymine is a kind of rich amine reagent, itself and cheap chitosan solution is blended, form three-dimensional network by simple chemical crosslinking to entwine structure, in cooperation, amido is to the strong complexing of iron ion, effectively can fix iron ion among microballoon by envelope, prevent its drop from going out, strengthen sorbent structure stability, and effectively retain the adsorption capacity of hydrated ferric oxide heavy metal anion; Meanwhile, the neutral amine of polymine and protonated amines also significantly can increase its adsorption site quantity to metal cation and anion; This preparation technology is simply effective, and the multi-functional compound adsorbent of preparation can work in coordination with trap heavy metals zwitterion by Large Copacity, has no relevant preparation and performance report at present;
(3) invention also provides a kind of method of N doping, effectively prevent the stripping of conventional iron embedding sorbing material iron in adsorption process, and neutral amine and the protonated amines of polyamines reagent can be utilized, improve the both sexes adsorption capacity of compound adsorbent further;
(4) composite adsorbing material prepared by the present invention can realize the collaborative removal of polluting metal anions and canons in same absorption system, and cheaper starting materials is easy to get, and preparation technology is simple, therefore can realize high environmental benefit under low input condition;
(5) the chitosan-based compound adsorbent prepared of the present invention is with low cost, and Stability Analysis of Structures, superior performance, can work in coordination with high efficiency synchronous removal heavy metal zwitterion, has broad application prospects in heavy metal zwitterion combined pollutant Collaborative Control.
Accompanying drawing explanation
Fig. 1 is the electromicroscopic photograph of shitosan base composite absorbent in the present invention, and wherein scheming (A) is SEM photo, and figure (B) is TEM photo.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is described further.
Embodiment 1
Work in coordination with a chitosan-based compound adsorbent for efficient removal heavy metal zwitterion, its synthesis step is:
A) accurately take 3g Chitosan powder to be added in the there-necked flask that 100mL distilled water is housed, then drip 2mL acetic acid in solution, at 60 DEG C of temperature, mechanical agitation 2h all dissolves to shitosan, obtains shitosan mother liquor.Measure 30mL shitosan mother liquor, add 0.4g ferric sulfate and 1g polymine wherein, normal temperature lower magnetic force is stirred to Homogeneous phase mixing, again gained homogeneous solution is transferred in there-necked flask, drip the epoxychloropropane of 0.25mL wherein, 60 DEG C of temperature lower magnetic forces stir 2h and are tentatively cross-linked, and obtain mixing mother liquor.
B) mixing mother liquor is pumped into 250mL to contain in the coagulating bath of 16g NaOH and 13g sodium sulphate and solidify balling-up, leave standstill 30min, filter out complex microsphere, clean and be placed in distilled water and preserve.
C) take 2g complex microsphere and be placed in the sodium hydrate aqueous solution that 100mLpH=13 is housed, drip the epoxychloropropane of 0.3mL wherein, add at 60 DEG C of temperature after thermal agitation 2h carries out and be cross-linked, take out thus obtained microsphere distilled water and be washed till neutrality, freeze-drying is preserved.Compound adsorbent called after A prepared by embodiment 1.
Embodiment 2
Work in coordination with a chitosan-based compound adsorbent for efficient removal heavy metal zwitterion, its synthesis step is:
A) accurately take 0.2g Chitosan powder to be added in the there-necked flask that 100mL distilled water is housed, then drip 1mL acetic acid in solution, at 20 DEG C of temperature, mechanical agitation 4h all dissolves to shitosan, obtains shitosan mother liquor.Measure 30mL shitosan mother liquor, add 0.15g ferric sulfate and 0.3g polymine wherein, normal temperature lower magnetic force is stirred to Homogeneous phase mixing, again gained homogeneous solution is transferred in there-necked flask, drip the epoxychloropropane of 0.15mL wherein, 80 DEG C of temperature lower magnetic forces stir 20h and are tentatively cross-linked, and obtain mixing mother liquor.
B) mixing mother liquor is pumped into 250mL to contain in the coagulating bath of 2.5g NaOH and 5g sodium sulphate and solidify balling-up, leave standstill 30min, filter out complex microsphere, clean and be placed in distilled water and preserve.
C) take 0.2g complex microsphere and be placed in the sodium hydrate aqueous solution that 100mLpH=14 is housed, drip the epoxychloropropane of 0.50mL wherein, add at 80 DEG C of temperature after thermal agitation 20h carries out and be cross-linked, take out thus obtained microsphere distilled water and be washed till neutrality, freeze-drying is preserved.Compound adsorbent called after B prepared by embodiment 2.
Embodiment 3
Work in coordination with a chitosan-based compound adsorbent for efficient removal heavy metal zwitterion, its synthesis step is:
A) accurately take 5g Chitosan powder to be added in the there-necked flask that 100mL distilled water is housed, then drip 8mL acetic acid in solution, at 80 DEG C of temperature, mechanical agitation 10h all dissolves to shitosan, obtains shitosan mother liquor.Measure 30mL shitosan mother liquor, add 1.8g ferric sulfate and 3g polymine wherein, normal temperature lower magnetic force is stirred to Homogeneous phase mixing, again gained homogeneous solution is transferred in there-necked flask, drip the epoxychloropropane of 1.20mL wherein, 20 DEG C of temperature lower magnetic forces stir 4h and are tentatively cross-linked, and obtain mixing mother liquor.
B) mixing mother liquor is pumped into 250mL to contain in the coagulating bath of 50g NaOH and 50g sodium sulphate and solidify balling-up, leave standstill 30min, filter out complex microsphere, clean and be placed in distilled water and preserve.
C) take 4g complex microsphere and be placed in the sodium hydrate aqueous solution that 100mLpH=10 is housed, drip the epoxychloropropane of 0.01mL wherein, add at 20 DEG C of temperature after thermal agitation 5h carries out and be cross-linked, take out thus obtained microsphere distilled water and be washed till neutrality, freeze-drying is preserved.Compound adsorbent called after C prepared by embodiment 3.
Embodiment 4
The basic step of the present embodiment is with embodiment 1, and difference is: by step B) in the dosage of ferric sulfate change 0.57g into.Compound adsorbent called after D prepared by embodiment 4.
Embodiment 5
The basic step of the present embodiment is with embodiment 1, and difference is: by step B) in the dosage of polymine change 1.5g into.Compound adsorbent called after E prepared by embodiment 5.
Embodiment 6
The basic step of the present embodiment is with embodiment 1, and difference is: by step B) in the consumption of epoxychloropropane change 0.3mL into, crosslinking temperature changes 80 DEG C into, and crosslinking time changes 3h into; Step D) in the consumption of epoxychloropropane change 0.4mL into, crosslinking temperature changes 80 DEG C into, and crosslinking time changes 3h into.Compound adsorbent called after F prepared by embodiment 6.
Embodiment 7
The basic step of the present embodiment is with embodiment 1, and difference is: by steps A) in the dosage of shitosan change 4g into.Compound adsorbent called after G prepared by embodiment 7.
Figure of description 1 is shown in by SEM and the TEM photo of the compound adsorbent prepared by embodiment 1.For the absorption property of research compound adsorbent heavy metal zwitterion, carry out following adsorption experiment, concrete adsorption conditions is: 0.025g adsorbent is placed in 50mL copper nitrate respectively, plumbi nitras, cadmium nitrate, potassium chromate, carry out single, double component absorption in Macquer's salt solution and between two mixed liquor, wherein the concentration of heavy metal anions and canons is 1mmol/L, initial pH is regulated to be 4.5, adsorption temp is 30 DEG C, and oscillation rate is 160r/min, and adsorption time is 24h.The adsorption capacity of single bi-component of compound adsorbent A ~ G heavy metal anions and canons of gained is in table 1.
Single Bicomponent Adsorption capacity of compound adsorbent heavy metal anions and canons in table 1 embodiment A ~ G
As can be seen from result, compound adsorbent heavy metal zwitterion one-component all shows very large adsorption capacity, in bi-component, the adsorbance of heavy metal zwitterion all comparatively has in one-component and significantly promotes even more noteworthy, illustrate in Bicomponent Adsorption process, heavy metal zwitterion has synergistic sorption effect, therefore this compound adsorbent metal zwitterion collaborative trapping and innoxious in there is very large application prospect.
In conjunction with the embodiments 1 ~ 7, adopt the chitosan-based compound adsorbent that preparation method provided by the invention synthesizes, efficient removal heavy metal zwitterion can be worked in coordination with.Preparation scheme provided by the invention is simply effective, with low cost, has broad application prospects in the common removal of Heavy Metals in Waters zwitterion pollutant.
Schematically above be described the present invention and embodiment thereof, this description does not have restricted, data used yet just one of embodiments of the present invention, actual data assemblies in being confined to this.So, if those of ordinary skill in the art enlightens by it, when not departing from the invention aim, without creatively designing the embodiment similar to this technical scheme and embodiment, all should protection scope of the present invention be belonged to.
Claims (9)
1. can work in coordination with a preparation method for the chitosan-based compound adsorbent of efficient removal heavy metal zwitterion, the steps include:
A) Chitosan powder be dissolved in acetic acid solution form shitosan mother liquor, in shitosan mother liquor, add ferric sulfate and polymine, stir, and just crosslinked with epoxychloropropane after obtain mixing mother liquor;
B) gained mixing mother liquor is added in coagulating bath, solidify through precipitation and obtain complex microsphere;
C) take out complex microsphere, be added in the aqueous solution of NaOH, carry out rear crosslinked with epoxychloropropane, obtained crosslinked microsphere, be washed till neutrality with distilled water, dehydrated preservation is for subsequent use.
2. a kind of preparation method working in coordination with the chitosan-based compound adsorbent of efficient removal heavy metal zwitterion according to claim 1, it is characterized in that: steps A) in shitosan mother liquor in, the mass concentration of shitosan is 2 ~ 50g/L, the volumetric concentration of acetic acid is 1 ~ 8%, solution temperature is 20 ~ 80 DEG C, and dissolution time is 2 ~ 10h.
3. a kind of preparation method working in coordination with the chitosan-based compound adsorbent of efficient removal heavy metal zwitterion according to claim 2, it is characterized in that: steps A) in the ferric sulfate that adds in shitosan mother liquor and polymine, make sulfuric acid iron speciation in mixing mother liquor be 5 ~ 60g/L, the mass concentration of polymine is 10 ~ 100g/L.
4. a kind of preparation method working in coordination with the chitosan-based compound adsorbent of efficient removal heavy metal zwitterion according to claim 3, it is characterized in that: steps A) in mixing mother liquor the volumetric concentration of crosslinking agent epoxychloropropane be 0.5 ~ 4%, crosslinking temperature is 20 ~ 80 DEG C, and crosslinking time is 2 ~ 20h.
5. a kind of preparation method working in coordination with the chitosan-based compound adsorbent of efficient removal heavy metal zwitterion according to claim 1, is characterized in that: step B) in coagulating bath used be the mixed solution being dissolved with in sodium sulphate, NaOH, sodium phosphate trimer and sodium pyrophosphate one or more.
6. a kind of preparation method working in coordination with the chitosan-based compound adsorbent of efficient removal heavy metal zwitterion according to claim 5, is characterized in that: step B) in coagulating bath used be the mixed aqueous solution that the mass concentration of NaOH and sodium sulphate is respectively 10 ~ 200g/L and 20 ~ 200g/L.
7. a kind of preparation method working in coordination with the chitosan-based compound adsorbent of efficient removal heavy metal zwitterion according to claim 1, it is characterized in that: described step C) in complex microsphere dosage be 2 ~ 40g/L, the pH of sodium hydrate aqueous solution is 10 ~ 14.
8. a kind of preparation method working in coordination with the chitosan-based compound adsorbent of efficient removal heavy metal zwitterion according to claim 7, it is characterized in that: described step C) reaction system in the volumetric concentration of epoxychloropropane be 0.01 ~ 0.5%, crosslinking temperature is 20 ~ 80 DEG C, and crosslinking time is 2 ~ 20h.
9. the chitosan-based compound adsorbent that a kind of preparation method working in coordination with the chitosan-based compound adsorbent of efficient removal heavy metal zwitterion in claim 1-8 described in any one prepares.
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