CN104383891B - Chitosan-pseudo boehmite doped magnetic adsorbent and preparation method thereof - Google Patents
Chitosan-pseudo boehmite doped magnetic adsorbent and preparation method thereof Download PDFInfo
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- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
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- B01J20/08—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04 comprising aluminium oxide or hydroxide; comprising bauxite
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Abstract
The invention provides a preparation method of a chitosan-pseudo boehmite doped magnetic adsorbent. The preparation method comprises the steps of preparation of a ferroferric oxide core, preparation of an ethanol solution of nano ferroferric oxide-isopropanol aluminum, preparation of a chitosan-acetic acid solution, preparation of the chitosan-pseudo boehmite doped magnetic adsorbent and the like. The invention also provides the chitosan-pseudo boehmite doped magnetic adsorbent which takes nano ferroferric oxide as the core, and doped with pseudo boehmite and crosslinked chitosan on the surface. The magnetic composite adsorbent prepared by the method has adsorption performance for cations and anions simultaneously, is large in adsorption capacity and high in moisture content, and has the advantages of high magnetism, stable properties, high mechanical properties and the like.
Description
Technical field
The invention belongs to material science and field of environment engineering, relate to one and heavy metal ion in subsoil water is had selectivity
Good, absorption property is good, the composite adsorbing material of repeatable utilization and preparation method thereof, aoxidize particularly to a kind of nanometer four
Three-iron is core, surface doping mimicry thin water aluminum and the sorbent preparation method of cross-linked chitosan.
Background technology
Subsoil water there are substantial amounts of heavy metal and fluorion, and its method for separating and concentrating is of a great variety, mainly have absorption method,
Chemical deposition method, electroosmose process, extraction, membrane process etc..
Absorption method is the most relatively inexpensive a kind of water processing mode, the active charcoal of common adsorbing material, activated alumina,
Nano ferriferrous oxide, chitosan etc..In existing report, mixing aluminum adsorbent is a kind of up-and-coming adsorbent,
It has the strongest electrical absorption property to fluorine, is widely used in water process because of its low cost, regenerating easily character again
(B.J.Ash, 2002).Some research worker are prepared for aluminum doped magnetic material (Yuanyuan Zheng, 2012), energy
Fluorion in enough effectively removal water bodys, but relatively low to the arsenic removal efficiency in water body, and there is the problem that aluminium ion runs off.
Utilize macromolecular material that dopant material is modified, adsorbing material performance can be effectively improved, and reduce aluminum ions loss.
But the material for macromolecular material and aluminum doping rarely has report (C.Sairam Sundaram, 2009).And at high score
In sub-material, chitosan is a kind of most suitable functional material, rich in-NH in its chemical constitution2With-OH, right
The metal ion of water body and anionic part have chelating adsorption (M.A.Morales, 2003).Such as, some grind
Study carefully librarian use aluminium compound and the polymer composite of chitosan synthesis, can effectively improve fluorine removal ability (N.
Viswanathan, 2010), and effectively stop metal ion to run off.But this AlCs composite absorption after be difficult to
Water body separates, and precipitation needs the long period.
Summary of the invention
Goal of the invention: in order to overcome above-mentioned the deficiencies in the prior art, it is an object of the invention to provide a kind of chitosan-mimicry
Thin water aluminum doped magnetic adsorbent and preparation method thereof, synthesis is a kind of thin with ferroso-ferric oxide surface covering chitosan and mimicry
The nano-particle of water aluminum mixture film.
Technical scheme: the preparation method of a kind of chitosan-mimicry thin water aluminum doped magnetic adsorbent that the present invention provides, including
Following steps:
(1) preparation of ferroso-ferric oxide core: by dispersed extremely to iron chloride, polyvinylpyrrolidone, anhydrous sodium acetate
In ethylene glycol, 160-200 DEG C of reaction 6-10h, obtain ferroso-ferric oxide core；
(2) preparation of the ethanol solution of nano ferriferrous oxide-aluminum isopropylate.: aluminum isopropylate. is scattered in ethanol, then adds
Enter ferroso-ferric oxide core, 50-70 DEG C of reaction 8-12h, obtain the ethanol solution of nano ferriferrous oxide-aluminum isopropylate.；
(3) configuration of chitosan-acetic acid solution: glacial acetic acid, chitosan and water are mixed, stands, obtains chitosan-acetic acid
Solution；
(4) preparation of chitosan-mimicry thin water aluminum doped magnetic adsorbent: chitosan-acetic acid solution is dropped to nanometer four oxygen
Change in the ethanol solution of three-iron-aluminum isopropylate., Hydrolysis At Room Temperature reaction 0.5-1h；Adjust pH to 10-12, add epoxy chlorine
Propane, 60-80 DEG C of reaction 2-4h, obtain chitosan-mimicry thin water aluminum doped magnetic adsorbent.
Step (1), iron chloride, polyvinylpyrrolidone, anhydrous acetic acid, the amount ratio of ethylene glycol sum are 2.0-4.0g:
2.0-3.0g:6.0-9.0g:80mL:.
In step (2), the consumption of ferroso-ferric oxide core in terms of iron chloride, aluminum isopropylate. and the matter of ferroso-ferric oxide core
Amount ratio is 0.2-1.0:2.0-4.0, and is dissolved in 100-300mL ethanol.
In step (3), the amount ratio of glacial acetic acid, chitosan and water is 1.0-5.0mL:0.5-3.0g:500mL.
In step (4), chitosan-acetic acid solution, nano ferriferrous oxide-aluminum isopropylate. ethanol solution and epoxychloropropane
Amount ratio be 30-60mL:100-300mL:5-15mL.
Present invention also offers a kind of chitosan-mimicry thin water aluminum doped magnetic adsorbent, described chitosan-mimicry thin water aluminum
Doped magnetic adsorbent with nano ferriferrous oxide as core, surface doping mimicry thin water aluminum and cross-linked chitosan.
This chitosan-mimicry thin water aluminum doped magnetic adsorbent is to be prepared by any one method of claim 1 to 5.
Beneficial effect: the magnetic composite adsorbent that provider's method of the present invention prepares has cation and Anion-adsorption simultaneously
Performance, adsorption capacity is big, moisture content is high, has the advantages such as magnetic is strong, stable in properties, mechanical performance are strong.
Specifically, the present invention, relative to prior art, has an advantage highlighted below:
(1) relative to prior art, chitosan-mimicry thin water aluminum doped magnetic adsorbent is to be carried for the first time in this invention
And.This adsorbent is core-shell structure, and the magnetic of its core is Fe3O4, watchcase is cross-linked chitosan and AlOOH mixes
Miscellaneous material；Nano ferriferrous oxide rich surface in adsorbent contains carbonyl, and it coordinates with chitosan, in co-absorbed water
Heavy metal ion, mimicry thin water aluminum has stronger adsorption to the fluorion in water body；Ingenious compound three kinds of the present invention
The ionic state pollutant in water can effectively be removed by material, have bigger saturation magnetization and specific surface area feature, again
Solid water can be accelerated by magnetic separation technique because of its Physical magnetic to separate, reduce adsorbing material loss in water body.
(2) method that the present invention provides actually uses hydrothermal synthesis method to prepare magnetic core and Hydrolyze method peplos two step prepares absorption
Agent, specifically includes hydro-thermal method and prepares super-paramagnetism nano magnetic fluid, the preparation of aluminum isopropylate .-ethanol solution and hydrolysis legal system
Standby three key steps of compound adsorbent.After aluminum isopropylate .-ethanol solution mixes with ferroso-ferric oxide, ferroso-ferric oxide table
Face carbonyl reacts with aluminum isopropylate., forms (Fe3O4)-R-O-Al-R composite construction；After adding chitosan aqueous solution,
Composite construction hydrolyzes, and chitosan rapidly with hydrolysis after composite construction chelate, formation (Fe3O4)
-R-O-Al-CS structure；With epoxychloropropane for cross-linking agent rock-steady structure, it is cross-linked to form (Fe3O4)-R-O-Al-CS-R
(wherein CS is chitosan) structure.The preparation method of this adsorbent is simple, it is not necessary to nitrogen protection and high-temperature firing,
Process stabilization is controlled, and the adsorbent mass prepared is stable, has good IP prospecting.
(3) present invention solve to add chitosan chelates ferric ions after aluminium salt by two-step synthesis method and make adsorbing material lose magnetic
The problem of property.The magnetic organic/inorganic composite material adsorbent of preparation can be widely applied for the huge sum of money such as arsenic from underwater, chromium
Belong to and the removal of fluorion, to realize the Efficient Development utilization of cheap natural resources.Program technique is simple, the suction of product
Attached functional, use and reclaim conveniently.
Accompanying drawing explanation
Fig. 1 is that the present invention verifies example 1X ray photoelectron spectroscopic analysis (XPS) figure；
Fig. 2 is that the present invention verifies example 1 transmission electron microscope (TEM) figure；
Fig. 3 is structure composition and the film chemical structure chart of adsorbent of the present invention.
Detailed description of the invention
Embodiment 1
Chitosan-mimicry thin water aluminum doped magnetic adsorbent, its preparation process is as follows:
(1) iron chloride (FeCl of 2.0g is weighed3·6H2O) it is distributed to uniformly in 80mL ethylene glycol make solution.
And it is sequentially added into PVP (2.00g) and anhydrous sodium acetate (7.20g) under agitation, stir into homogeneous system.Will
This mixture is transferred in the 100mL reactor with politef lining seal, and finally autoclave is placed in electricity
Hot blast drying baker is heated to 180 DEG C and isothermal reaction 8h.After cooling, gained suspension Magneto separate is obtained black
Powdered substance.After spending this powder of absolute ethanol washing 3 times, transfer in 50mL volumetric flask with ethanol for medium,
It is settled to 50mL with ethanol.Obtain super-paramagnetism nano magnetic fluid.
(2) weigh 1.0g aluminum isopropylate. to be dissolved in 300mL dehydrated alcohol, ultrasonic 2h at 60 DEG C；By in above-mentioned (1)
50mL magnetic fluid mix with aluminum isopropylate ./ethanol solution, and ultrasonic to homogeneous system at 60 DEG C, transfer to close
In system, 60 DEG C of stirring reaction 10h, obtain nano ferriferrous oxide/aluminum isopropylate ./ethanol solution.
(3) taking 1.0mL glacial acetic acid and transfer in volumetric flask, the 500mL that adds water is configured to acetic acid solution.Weigh 0.5g
Chitosan, is transferred in above-mentioned acetic acid solution, is stirred until homogeneous state, stands overnight, obtain chitosan/acetic acid solution.
(4) 300mL nano ferriferrous oxide/aluminum isopropylate ./ethanol solution is transferred in there-necked flask, at 800rmp
Under stirring condition, the 30mL chitosan/acetic acid solution being slowly added dropwise in above-mentioned (3), continues stirring 1h.Drip dense ammonia
Water regulation pH to 10, adds 10mL epoxychloropropane, 70 DEG C of stirring 3h.After reaction terminates, under outside magnetic field effect
Collect product, after deionized water and dehydrated alcohol respectively washed product 3 times, be stored in 50mL water.
By the operation instruction of adsorbent prepared by this method: the liquid dispersion of adsorbent will be stocked uniformly before using, take certain
The adsorbent stock solution of amount, goals of investment is processed in water body, stirs certain time, separated by Magnet, and supernatant is
Process gained.
Embodiment 1 checking is shown in Table 1, Fig. 1 to Fig. 2.
Table 1 embodiment 1 verifies data
| Project | Data |
| Outward appearance | Dark grey flour |
| Iron-holder | 3.05% |
| Aluminum content | 15.65% |
| Bead particle diameter | 200-300nm |
| Saturation magnetization | 39.21emu/g |
| Fluorine saturated adsorption capacity | 72.3mg/g |
| Arsenic saturated adsorption capacity | 52.9mg/g |
Fig. 1 is X-ray photoelectron spectroscopic analysis (XPS) figure of checking example 1, and Fig. 2 is the transmission electron microscope of checking example 1
(TEM) figure.
Fig. 1 is X-ray photoelectron spectroscopic analysis, and as can be seen from the figure magnetic core is Fe3O4(non-γ-Fe2O3),
N, the Al contained in material is respectively from the cross-linked chitosan on top layer and AlOOH.
Fig. 2 is the TEM figure of material under transmission electron microscope, and as can be seen from the figure material is the uniform of 200-300nm particle diameter
Bead, and material surface is covered with a tunic, can show that it is cross-linked chitosan and AlOOH doping in conjunction with Fig. 1
Top layer film.
Embodiment 2
Chitosan-mimicry thin water aluminum doped magnetic adsorbent, its preparation process is as follows:
(1) iron chloride (FeCl of 3.0g is weighed3·6H2O) it is distributed to uniformly in 80mL ethylene glycol make solution.
And it is sequentially added into PVP (3.0g) and anhydrous sodium acetate (9.0g) under agitation, stir into homogeneous system.By this
Mixture is transferred in the 100mL reactor with politef lining seal, and finally autoclave is placed in electric heating
Air dry oven is heated to 200 DEG C and isothermal reaction 10h.After cooling, gained suspension Magneto separate is obtained black
Powdered substance.After spending this powder of absolute ethanol washing 3 times, transfer in 50mL volumetric flask with ethanol for medium,
It is settled to 50mL with ethanol.Obtain super-paramagnetism nano magnetic fluid.
(2) weigh 1.0g aluminum isopropylate. to be dissolved in 150mL dehydrated alcohol, ultrasonic to homogeneous system at 70 DEG C；By upper
The 50mL magnetic fluid stated in (1) mixes with aluminum isopropylate ./ethanol solution, and ultrasonic to homogeneous system at 70 DEG C, turns
Move on to 70 DEG C of stirring reaction 8h in closed system, obtain nano ferriferrous oxide/aluminum isopropylate ./ethanol solution.
(3) taking 3.0mL glacial acetic acid and transfer in volumetric flask, the 500mL that adds water is configured to acetic acid solution.Weigh 2.0g
Chitosan, is transferred in above-mentioned acetic acid solution, is stirred until homogeneous state, stands overnight, obtain chitosan/acetic acid solution.
(4) 150mL nano ferriferrous oxide/aluminum isopropylate ./ethanol solution is transferred in there-necked flask, at 800rmp
Under stirring condition, the 45mL chitosan/acetic acid solution being slowly added dropwise in above-mentioned (3), continues stirring 1h.Drip dense ammonia
Water regulation pH to 10, adds 5mL epoxychloropropane, 70 DEG C of stirring 3h.After reaction terminates, under outside magnetic field effect
Collect product, after deionized water and dehydrated alcohol respectively washed product 3 times, be stored in 50mL water.
By the operation instruction of adsorbent prepared by this method: the liquid dispersion of adsorbent will be stocked uniformly before using, take certain
The adsorbent stock solution of amount, goals of investment is processed in water body, stirs certain time, separated by Magnet, and supernatant is
Process gained.
Table 2 embodiment 2 verifies data
| Project | Data |
| Outward appearance | Dark grey flour |
| Iron-holder | 4.85% |
| Aluminum content | 16.85% |
| Bead particle diameter | 300-500nm |
| Saturation magnetization | 43.58emu/g |
| Fluorine saturated adsorption capacity | 79.1mg/g |
| Arsenic saturated adsorption capacity | 46.2mg/g |
X-ray photoelectron spectroscopic analysis (XPS) figure, transmission electron microscope (TEM) figure are consistent with embodiment 1.
Embodiment 3
Chitosan-mimicry thin water aluminum doped magnetic adsorbent, its preparation process is as follows:
(1) iron chloride (FeCl of 4.0g is weighed3·6H2O) it is distributed to uniformly in 80mL ethylene glycol make solution.
And it is sequentially added into PVP (3.0g) and anhydrous sodium acetate (6.0g) under agitation, stir into homogeneous system.By this
Mixture is transferred in the 100mL reactor with politef lining seal, and finally autoclave is placed in electric heating
Air dry oven is heated to 160 DEG C and isothermal reaction 6h.After cooling, gained suspension Magneto separate is obtained the powder of black
Powder material.After spending this powder of absolute ethanol washing 3 times, transfer in 50mL volumetric flask with ethanol for medium, use
Ethanol is settled to 50mL.Obtain super-paramagnetism nano magnetic fluid.
(2) weigh 0.2g aluminum isopropylate. to be dissolved in 150mL dehydrated alcohol, ultrasonic to homogeneous system at 70 DEG C；By upper
The 50mL magnetic fluid stated in (1) mixes with aluminum isopropylate ./ethanol solution, and ultrasonic to homogeneous system at 70 DEG C, turns
Move on to 80 DEG C of stirring reaction 12h in closed system, obtain nano ferriferrous oxide/aluminum isopropylate ./ethanol solution.
(3) taking 5.0mL glacial acetic acid and transfer in volumetric flask, the 500mL that adds water is configured to acetic acid solution.Weigh 3.0g
Chitosan, is transferred in above-mentioned acetic acid solution, is stirred until homogeneous state, stands overnight, obtain chitosan/acetic acid solution.
(4) 100mL nano ferriferrous oxide/aluminum isopropylate ./ethanol solution is transferred in there-necked flask, at 800rmp
Under stirring condition, the 60mL chitosan/acetic acid solution being slowly added dropwise in above-mentioned (3), continues stirring 1h.Drip dense ammonia
Water regulation pH to 10, adds 15mL epoxychloropropane, 70 DEG C of stirring 3h.After reaction terminates, under outside magnetic field effect
Collect product, after deionized water and dehydrated alcohol respectively washed product 3 times, be stored in 50mL water.
By the operation instruction of adsorbent prepared by this method: the liquid dispersion of adsorbent will be stocked uniformly before using, take certain
The adsorbent stock solution of amount, goals of investment is processed in water body, stirs certain time, separated by Magnet, and supernatant is
Process gained.
Table 3 embodiment 3 verifies data
| Project | Data |
| Outward appearance | Dark grey flour |
| Iron-holder | 4.85% |
| Aluminum content | 16.85% |
| Bead particle diameter | 300-500nm |
| Saturation magnetization | 43.58emu/g |
| Fluorine saturated adsorption capacity | 79.1mg/g |
| Arsenic saturated adsorption capacity | 46.2mg/g |
X-ray photoelectron spectroscopic analysis (XPS) figure, transmission electron microscope (TEM) figure are consistent with embodiment 1.
Claims (6)
1. the preparation method of chitosan-mimicry thin water aluminum doped magnetic adsorbent, it is characterised in that: include
Following steps:
(1) preparation of ferroso-ferric oxide core: by uniform to iron chloride, polyvinylpyrrolidone, anhydrous sodium acetate
It is dispersed in ethylene glycol, 160-200 DEG C of reaction 6-10h, obtains ferroso-ferric oxide core；
(2) preparation of the ethanol solution of nano ferriferrous oxide-aluminum isopropylate.: aluminum isopropylate. is scattered in ethanol
In, add ferroso-ferric oxide core, 50-70 DEG C of reaction 8-12h, obtain nano ferriferrous oxide-isopropanol
The ethanol solution of aluminum；
(3) configuration of chitosan-acetic acid solution: glacial acetic acid, chitosan and water are mixed, stands, obtains shell
Polysaccharide-acetic acid solution；
(4) preparation of chitosan-mimicry thin water aluminum doped magnetic adsorbent: by chitosan-acetic acid solution dropping
To the ethanol solution of nano ferriferrous oxide-aluminum isopropylate., Hydrolysis At Room Temperature reaction 0.5-1h；Adjust pH extremely
10-12, adds epoxychloropropane, 60-80 DEG C of reaction 2-4h, obtains chitosan-mimicry thin water aluminum doping magnetic
Property adsorbent.
The preparation of a kind of chitosan-mimicry the most according to claim 1 thin water aluminum doped magnetic adsorbent
Method, it is characterised in that: in step (1), iron chloride, polyvinylpyrrolidone, anhydrous sodium acetate, second two
The amount ratio of alcohol is 2.0-4.0g:2.0-3.0g:6.0-9.0g:80mL.
The preparation of a kind of chitosan-mimicry the most according to claim 1 thin water aluminum doped magnetic adsorbent
Method, it is characterised in that: in step (2), the consumption of ferroso-ferric oxide core in terms of iron chloride, aluminum isopropylate.
It is 0.2-1.0:2.0-4.0 with the mass ratio of ferroso-ferric oxide core, is dissolved in 100-300mL ethanol.
The preparation of a kind of chitosan-mimicry the most according to claim 1 thin water aluminum doped magnetic adsorbent
Method, it is characterised in that: in step (3), the amount ratio of glacial acetic acid, chitosan and water is 1.0-5.0mL:
0.5-3.0g:500mL.
The preparation of a kind of chitosan-mimicry the most according to claim 1 thin water aluminum doped magnetic adsorbent
Method, it is characterised in that: in step (4), chitosan-acetic acid solution, nano ferriferrous oxide-isopropanol
The amount ratio of aluminum ethanol solution and epoxychloropropane is 30-60mL:100-300mL:5-15mL.
6. chitosan-mimicry thin water aluminum doped magnetic adsorbent, it is characterised in that: described chitosan-plan
State thin water aluminum doped magnetic adsorbent with nano ferriferrous oxide as core, surface doping mimicry thin water aluminum and crosslinking shell
Polysaccharide；It is to be prepared by any one method of claim 1 to 5.
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