CN109174041A - A kind of preparation and its application of removal Cu (II) in water of the porous trace hydrogel of GO-CS - Google Patents
A kind of preparation and its application of removal Cu (II) in water of the porous trace hydrogel of GO-CS Download PDFInfo
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- CN109174041A CN109174041A CN201811219640.6A CN201811219640A CN109174041A CN 109174041 A CN109174041 A CN 109174041A CN 201811219640 A CN201811219640 A CN 201811219640A CN 109174041 A CN109174041 A CN 109174041A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- 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
- B01J20/26—Synthetic macromolecular compounds
- B01J20/268—Polymers created by use of a template, e.g. molecularly imprinted polymers
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
- B01J20/28047—Gels
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/305—Addition of material, later completely removed, e.g. as result of heat treatment, leaching or washing, e.g. for forming pores
- B01J20/3057—Use of a templating or imprinting material ; filling pores of a substrate or matrix followed by the removal of the substrate or matrix
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/288—Treatment of water, waste water, or sewage by sorption using composite sorbents, e.g. coated, impregnated, multi-layered
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
Abstract
The present invention relates to the preparation methods that a kind of preparation method of aquagel more particularly to a kind of chitosan multi-porous trace hydrogel of graphene oxide-remove Cu (II) in water removal for this.Belong to material preparation and separation technology field.Refer in particular to that there is porous blotting chitosan hydrogel with prepared by phase separation method and ionic imprinting technique by crosslinking-oxidization graphene, and for the adsorption recovery to divalent heavy metal Cu.The absorption property of this material is had studied by adsorption experiment.The result shows that there is superior absorption property using the porous blotting chitosan hydrogel that the present invention obtains.
Description
Technical field
The present invention relates to a kind of preparation method of aquagel more particularly to a kind of graphene oxide-chitosan are more
Hole trace hydrogel goes the preparation method of Cu (II) in water removal.Belong to material preparation and separation technology field.
Background technique
Copper (Cu) is intermetallic composite coating, machine-building, the primary pollution source of steel production etc..The toxicity for drinking rear human body is put
More toxic organic compound matter are generated greatly and in conjunction with other toxin in water.So far, in aqueous solution Cu (II) processing side
Method includes chemical precipitation, redox, solvent extraction, absorption etc..In these methods, absorption is considered most fast and most effective
One of method.Active carbon is the most common adsorbent for removing removing heavy metals, but active carbon has many limitations and is easy
Lead to secondary pollution.Bacterium, yeast and Mold adsorbent have poor mechanical stability, weaker target adsorptive selectivity and compared with
The slow rate of adsorption.
Graphene oxide (GO) is a kind of new carbon haveing excellent performance, and specific surface area with higher and surface are abundant
Functional group.Ionic imprinting technique selects suitable function monomer, crosslinking agent and polymerization side using anions and canons as template ion
Formula is polymerize in aqueous solution, and ion after removing template is gone just to obtain the ion blotting polymerization of specific hole size and shape
Object.The advantages that affinity strong, the selectivity height of ion imprinted polymer, anti-adverse environment, stability is good, long service life,
It is generally applied to the separation and removal of heavy metal ions in wastewater.It is more that chitosan (CS) is found to be unique natural cationic
Sugar.Its biomass is very big, is the deacetylated product of chitin, so the macromolecular of chitosan has active hydroxyl and ammonia
Base, they have very strong chemical reaction ability.Chitosan has unique physicochemical properties, such as adsorbs, film forming, fiber shape
At moisture absorption and moisturizing.As the utilization of resources, chitosan has abundant raw material, and regeneration is fast, environmental-friendly, good biocompatibility etc.
Feature, the processing to water pollution, the especially absorption of heavy metal ion in water are also of great significance.
Summary of the invention
The present invention is the chitosan product with porous imprinted structures and pattern directly to be prepared by phase separation method, and be used for
To the adsorption recovery of divalent heavy metal Cu.
The technical scheme is that
It is a kind of adsorb divalent heavy metal Cu the chitosan multi-porous trace hydrogel of graphene oxide-preparation method, by with
Lower step carries out:
(1) a certain amount of graphene oxide is taken to be placed in a beaker；
(2) it takes a certain amount of glacial acetic acid to be added in the beaker of step (1), and stirs evenly；
(3) a certain amount of chitosan is added in the solution of step (2), stirring evenly 15min and being ultrasonically treated 1h makes it
It mixes well；
(4) a certain amount of Gerhardite is added into the mixed solution of step (3), stirs evenly；
(5) above-mentioned beaker is placed on blender, is separately added into a certain amount of carbodiimide and N- hydroxyl while stirring
Succinimide；
(6) refrigerator overnight is put into after the solution that step (5) obtain being placed 1h at 25 DEG C；
(7) solution after staying overnight step (6) is freeze-dried 48h through certain temperature；
(8) hydrogel after being lyophilized is lyophilized for 24 hours again after being washed with distilled water, this process is repeated several times.
Wherein, in graphene oxide described in step (1) mass percent of graphene in aqueous solution be 0.3~
0.5%.
Wherein, the mass percent in entire solution of glacial acetic acid described in step (2) is 0.5~1.5%.
Wherein, the dosage of chitosan described in step (3) is 1.8~2.2g.
Wherein, mass percent is 0.8~1.2% to Gerhardite described in step (4) in the solution.
Wherein, carbodiimide mass percent described in step (5) is 1.5~2.5%.
Wherein, n-hydroxysuccinimide mass percent described in step (5) is 0.2~0.35%.
Wherein, the temperature of freeze-drying described in step (7) is -45~-60 DEG C.
Wherein, the number for washing hydrogel described in step (8) repeatedly is 3~5 times.
The above-mentioned chitosan multi-porous trace hydrogel (GO-IICCS) of graphene oxide-is applied to absorption divalent heavy metal Cu,
Specific method carries out as steps described below:
(1) pH: being respectively the Cu stock solution of 2.0,4.0,5.0,6.0 and 7.0 by 10mg GO-IICCS immersion pH
(10mL,50mg L-1) in, for 24 hours, (passing through flame atomic absorption spectrophotometer) measures the ultimate density of Cu (II) for reaction.Examination
The pH value for testing middle Cu (II), which is adjusted, uses 0.1M NaOH and 0.1M HCl solution.
(2) under conditions of 298K, 10mg GO-IICCS adsorption dynamics adsorption kinetics: is immersed in 10ml Cu (II) stock solution
(50mg L-1, pH=7.0) in.Contact 1-960min is tested.The residual concentration of Cu (II) is divided light by Flame Atomic Absorption Spectrometry
Degree meter measurement.
(3) 10mg GO-IICCS adsorption isotherm: is immersed into various concentration Cu (II) stock solution (10ml, pH=7.0)
In, Cu (II) solution concentration is respectively 10,25,50,75,100,150,200,250 and 300mg L-1.Pass through Flame Atomic Absorption Spectrometry
Spectrophotometer detects residual concentration.
(4) 10mg GO-IICCS Adsorption thermodynamics: is immersed into 10ml Cu (II) stock solution (50mg L-1, pH=7.0)
For 24 hours, reaction temperature is respectively 298,308,318 and 323K for middle reaction.It is detected and is remained by flame atomic absorption spectrophotometer
Concentration.
(5) competitive Adsorption: preparation Cu (II), Cr (III), Pb (II) and (II) four kind of concentration of Zn are 50mg L-1Ion
10mg GO-IICCS is immersed in reaction in the above-mentioned mixed solution of 10ml (pH=7.0) under conditions of 298K by mixed solution
24h.Residual concentration is detected finally by flame atomic absorption spectrophotometer.
(6) repeated experiment: will be 50mg L in pH=7.0,298K and Cu (II) stock concentrations-1Under the conditions of it is anti-
The hydrogel answered is collected, and is eluted completely, then adsorbed under the same conditions with acetum (1:9), is passed through Flame Atomic Absorption Spectrometry
Spectrophotometer detects residual concentration, which is repeated 5 times.
Above-mentioned steps (1) obtain the amount of GO-IICCS removal Cu (II) in balance in pH=2.0,4.0,5.0,6.0 and
7.0 be respectively 32.61,33.13,35.22,36.71 and 39.28mg g-1。
Above-mentioned steps (2) show that the dynamics of GO-IICCS removal Cu (II) and pseudo-second order kinetic model more meet (R2
=0.996).
Above-mentioned steps (3) obtain GO-IICCS to the saturated extent of adsorption 76.35mg g of Cu (II)-1。
Above-mentioned steps (4) show that GO-IICCS is 323K for Cu (II) optimum temperature adsorbed, due to chitosan itself
Heat resistance it is bad, so not considering the experiment of higher temperature.
Above-mentioned steps (5) show that GO-IICCS has specific selection adsorption capacity for Cu (II).
Above-mentioned steps (6) show that GO-IICCS after 5 times recycle, still remains 81% adsorption capacity.
Technological merit of the invention:
(1) by phase separation method, addition graphene oxide directly prepares the aquagel with porous imprinted structures.
(2) GO-IICCS is made to have specific selection adsorption capacity to Cu (II) using ionic imprinting technique.
Detailed description of the invention
The scanning electron microscope image of Fig. 1 .GO-IICCS
Fourier-transform infrared (FT-IR) spectrogram of Fig. 2 .GO-IICCS
Specific embodiment
Below with reference to specific implementation example, the present invention will be further described.
(9) embodiment 1: taking 50mL concentration is 1.5mg mL-1Graphene oxide solution in 100mL beaker, be added
It is mixed after 0.24mL glacial acetic acid, then 1.8g chitosan is added into beaker, stirred 15min and being ultrasonically treated 1h keeps its mixing equal
It is even.0.4g Gerhardite is added into beaker to be uniformly mixed, places the beaker and 0.75g carbon is added on blender while stirring
Diimine and 0.1gN- HOSu NHS are put into refrigerator overnight after placing 1h at 25 DEG C after mixing.After overnight
- 45 DEG C of freeze-drying 48h of solution warp.Hydrogel after freeze-drying is lyophilized for 24 hours again after being washed with distilled water, and this process 3 times repeatedly.
Embodiment 2: taking 50mL concentration is 2mg mL-1Graphene oxide solution in 100mL beaker, be added 0.48mL ice
It is mixed after acetic acid, then 2g chitosan is added into beaker, stirred 15min and being ultrasonically treated 1h is uniformly mixed it.Into beaker
Be added 0.5g Gerhardite be uniformly mixed, place the beaker be added while stirring on blender 0.96g carbodiimide and
0.14gN- HOSu NHS is put into refrigerator overnight after placing 1h at 25 DEG C after mixing.Solution warp-after overnight
50 DEG C of freeze-drying 48h.Hydrogel after freeze-drying is lyophilized for 24 hours again after being washed with distilled water, and this process 4 times repeatedly.
Embodiment 3: taking 50mL concentration is 2.5mg mL-1Graphene oxide solution in 100mL beaker, be added 0.96mL
It is mixed after glacial acetic acid, then 2.2g chitosan is added into beaker, stirred 15min and being ultrasonically treated 1h is uniformly mixed it.To burning
0.6g Gerhardite is added in cup to be uniformly mixed, places the beaker and 1.25g carbodiimide is added on blender while stirring
With 0.175gN- HOSu NHS, refrigerator overnight is put into after placing 1h at 25 DEG C after mixing.Solution after overnight
Through -60 DEG C of freeze-drying 48h.Hydrogel after freeze-drying is lyophilized for 24 hours again after being washed with distilled water, and this process 5 times repeatedly.
As shown in Figure 1, after crosslinking Treatment, the GO-IICCS bracket of preparation is porous structure.SEM image shows that height is more
Hole and structure interconnected, while GO-IICCS bracket shows the micro-structure folded and uneven surface.
As shown in Figure 2, in order to confirm the chemical structure of bracket, FTIR spectrum is measured.The assymmetrical deformation of amido protonation
Vibrate (- NH3 +, 1597cm-1) and aromatic amine (- CN, 1325cm-1) stretching vibration show that amino is present in chitosan.Acyl
Amine I (1648cm-1) stretching vibration and amide II (1590cm-1) bending vibration show propping up due to chemical crosslink reaction
Amido bond (- NHCO -) is formd in frame.Since the GO concentration being incorporated in chitosan stent is low (0.2%W/V), FTIR light
Spectrum can not identify the presence of GO in GO-IICCS bracket.
It can be seen that by experimental result above and graphene oxide and ion blotting preparation height added by phase separation method
Performance aquagel, to adsorb the Cu in water (II).By the analysis to pattern and functional group, the more of hydrogel are demonstrated
Layer porous structure.Since GO-IICCS has porous structure, the mass-transfer efficiency of adsorption process is improved, to make material
Adsorption efficiency is high, and adsorption capacity is big.GO-IICCS maximum adsorption capacity is 76.35mg g-1.Due to being added to ion blotting skill
Art, GO-IICCS have very strong selective adsorption capacity to Cu (II).After the regeneration that five recycle, adsorption capacity is still protected
Hold up to 81%.The advantages that GO-IICCS also has hydrophily strong, firm in structure, and stability is good, recoverable has very big
Prospects for commercial application.
Claims (9)
1. a kind of preparation method for the chitosan multi-porous trace hydrogel of graphene oxide-for adsorbing divalent heavy metal Cu, by following
Step carries out:
(1) a certain amount of graphene oxide is taken to be placed in a beaker；
(2) it takes a certain amount of glacial acetic acid to be added in the beaker of step (1), and stirs evenly；
(3) a certain amount of chitosan is added in the solution of step (2), stirring evenly 15min and being ultrasonically treated 1h makes it sufficiently
It mixes；
(4) a certain amount of Gerhardite is added into the mixed solution of step (3), stirs evenly；
(5) above-mentioned beaker is placed on blender, is separately added into a certain amount of carbodiimide and N- hydroxysuccinimidyl while stirring
Acid imide；
(6) refrigerator overnight is put into after the solution that step (5) obtain being placed 1h at 25 DEG C；
(7) solution after staying overnight step (6) is freeze-dried 48h through certain temperature；
(8) hydrogel after being lyophilized is lyophilized for 24 hours again after being washed with distilled water, this process is repeated several times.
2. a kind of absorption divalent heavy metal Cu graphene oxide-chitosan multi-porous trace hydrogel according to claim 1
Preparation method, which is characterized in that the mass percent of graphene in aqueous solution is in graphene oxide described in step (1)
0.3~0.5%.
3. a kind of absorption divalent heavy metal Cu graphene oxide-chitosan multi-porous trace hydrogel according to claim 1
Preparation method, which is characterized in that glacial acetic acid described in step (2) in entire solution mass percent be 0.5~1.5%.
4. a kind of absorption divalent heavy metal Cu graphene oxide-chitosan multi-porous trace hydrogel according to claim 1
Preparation method, which is characterized in that the dosage of chitosan described in step (3) be 1.8~2.2g.
5. a kind of absorption divalent heavy metal Cu graphene oxide-chitosan multi-porous trace hydrogel according to claim 1
Preparation method, which is characterized in that Gerhardite described in step (4) in the solution mass percent be 0.8~
1.2%.
6. a kind of absorption divalent heavy metal Cu graphene oxide-chitosan multi-porous trace hydrogel according to claim 1
Preparation method, which is characterized in that carbodiimide mass percent described in step (5) be 1.5~2.5%.
7. a kind of absorption divalent heavy metal Cu graphene oxide-chitosan multi-porous trace hydrogel according to claim 1
Preparation method, which is characterized in that n-hydroxysuccinimide mass percent described in step (5) be 0.2~0.35%.
8. a kind of absorption divalent heavy metal Cu graphene oxide-chitosan multi-porous trace hydrogel according to claim 1
Preparation method, which is characterized in that the temperature range of freeze-drying described in step (7) be -45~-60 DEG C.
9. a kind of absorption divalent heavy metal Cu graphene oxide-chitosan multi-porous trace hydrogel according to claim 1
Preparation method, which is characterized in that described in step (8) repeatedly wash hydrogel number be 3~5 times.
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| CN111068632A (en) * | 2020-01-23 | 2020-04-28 | 福州大学 | Lead ion composite adsorbent and preparation method thereof |
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Application publication date: 20190111 |