CN115155531B - polyaniline/Fe 3 O 4 CuO fiber and preparation method and application thereof - Google Patents
polyaniline/Fe 3 O 4 CuO fiber and preparation method and application thereof Download PDFInfo
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- 229920000767 polyaniline Polymers 0.000 title claims abstract description 92
- 239000000835 fiber Substances 0.000 title claims abstract description 82
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 238000001179 sorption measurement Methods 0.000 claims abstract description 56
- -1 halogen ions Chemical class 0.000 claims abstract description 47
- 229910052736 halogen Inorganic materials 0.000 claims abstract description 35
- 239000007864 aqueous solution Substances 0.000 claims abstract description 25
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000002791 soaking Methods 0.000 claims abstract description 17
- 239000003999 initiator Substances 0.000 claims abstract description 12
- 238000002156 mixing Methods 0.000 claims abstract description 12
- 239000002253 acid Substances 0.000 claims abstract description 11
- 230000001105 regulatory effect Effects 0.000 claims abstract description 7
- 238000006243 chemical reaction Methods 0.000 claims abstract description 3
- 239000007788 liquid Substances 0.000 claims abstract description 3
- 239000007787 solid Substances 0.000 claims abstract 2
- 239000000243 solution Substances 0.000 claims description 14
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- JOXIMZWYDAKGHI-UHFFFAOYSA-N toluene-4-sulfonic acid Chemical compound CC1=CC=C(S(O)(=O)=O)C=C1 JOXIMZWYDAKGHI-UHFFFAOYSA-N 0.000 claims description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 4
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 4
- 239000012670 alkaline solution Substances 0.000 claims description 3
- LCPVQAHEFVXVKT-UHFFFAOYSA-N 2-(2,4-difluorophenoxy)pyridin-3-amine Chemical compound NC1=CC=CN=C1OC1=CC=C(F)C=C1F LCPVQAHEFVXVKT-UHFFFAOYSA-N 0.000 claims description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 2
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 2
- 229910017604 nitric acid Inorganic materials 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Substances [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 claims description 2
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 21
- CPELXLSAUQHCOX-UHFFFAOYSA-M Bromide Chemical compound [Br-] CPELXLSAUQHCOX-UHFFFAOYSA-M 0.000 description 16
- 230000000052 comparative effect Effects 0.000 description 11
- 238000000034 method Methods 0.000 description 10
- 239000003463 adsorbent Substances 0.000 description 9
- 230000000694 effects Effects 0.000 description 8
- 229910052740 iodine Inorganic materials 0.000 description 8
- 239000011630 iodine Substances 0.000 description 8
- 238000005406 washing Methods 0.000 description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 8
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 7
- 239000003513 alkali Substances 0.000 description 7
- 229940006460 bromide ion Drugs 0.000 description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- 150000002367 halogens Chemical class 0.000 description 6
- 239000002244 precipitate Substances 0.000 description 6
- 229910052731 fluorine Inorganic materials 0.000 description 5
- 239000011737 fluorine Substances 0.000 description 5
- 239000000706 filtrate Substances 0.000 description 4
- XMBWDFGMSWQBCA-UHFFFAOYSA-M iodide Chemical compound [I-] XMBWDFGMSWQBCA-UHFFFAOYSA-M 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 3
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 description 3
- 229910052794 bromium Inorganic materials 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 229940006461 iodide ion Drugs 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 2
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 2
- NIPNSKYNPDTRPC-UHFFFAOYSA-N N-[2-oxo-2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 NIPNSKYNPDTRPC-UHFFFAOYSA-N 0.000 description 2
- 125000003277 amino group Chemical group 0.000 description 2
- 229910052801 chlorine Inorganic materials 0.000 description 2
- 239000000460 chlorine Substances 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 125000001841 imino group Chemical group [H]N=* 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000010865 sewage Substances 0.000 description 2
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 1
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 238000009297 electrocoagulation Methods 0.000 description 1
- 238000000909 electrodialysis Methods 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- FWFGVMYFCODZRD-UHFFFAOYSA-N oxidanium;hydrogen sulfate Chemical compound O.OS(O)(=O)=O FWFGVMYFCODZRD-UHFFFAOYSA-N 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000001223 reverse osmosis Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
Classifications
-
- 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
- B01J20/262—Synthetic macromolecular compounds obtained otherwise than by reactions only involving carbon to carbon unsaturated bonds, e.g. obtained by polycondensation
-
- 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
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0233—Compounds of Cu, Ag, Au
- B01J20/0237—Compounds of Cu
-
- 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
- B01J20/06—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
- 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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- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention discloses polyaniline/Fe 3 O 4 CuO fiber, polyaniline/Fe 3 O 4 The CuO fibers are interlaced with each other to form clusters having a cage-like structure. The invention also discloses the polyaniline/Fe 3 O 4 The preparation method of the CuO fiber comprises the following steps: nano Fe 3 O 4 Mixing nano CuO with aniline, soaking, adding protonic acid aqueous solution, mixing, regulating temperature, dripping initiator aqueous solution, maintaining the temperature for reaction, and separating solid from liquid to obtain polyaniline/Fe 3 O 4 CuO fiber. The invention also discloses the polyaniline/Fe 3 O 4 Use of CuO fibers for adsorbing halogen ions. The invention has good adsorption performance to halogen ions.
Description
Technical Field
The invention relates to the technical field of adsorbents, in particular to polyaniline/Fe 3 O 4 CuO fiber and its preparation method and application are provided.
Background
The halogen elements include fluorine, chlorine, bromine and iodine. The halogen element is widely applied to industrial production, so that the sewage contains fluorine, chlorine, bromine and iodine ions, and the halogen element has toxicity and is easy to pollute the environment, thereby threatening the safety of people. Thus, it is necessary to remove halogen elements from the sewage.
The current methods for removing halogen elements include precipitation, evaporation and concentration, membrane separation, adsorption, electrolysis, electrocoagulation, electrodialysis, reverse osmosis, ion exchange, etc. The adsorption method has the advantages of high removal rate, simple process, reproducibility and the like, and has good industrial application prospect.
Polyaniline has special electrical, optical and adsorption properties. The polyaniline prepared at present has various forms and different adsorption performances, but the polyaniline is commonly used for adsorbing heavy metals and organic dyes. Polyaniline has little research on adsorption of halogen elements, and polyaniline is generally used on electrodes, and adsorption is performed by utilizing its electrical properties.
Disclosure of Invention
Based on the technical problems existing in the background technology, the invention provides a polyaniline/Fe 3 O 4 CuO fiber, preparation method and application thereof, and polyaniline/Fe prepared by the method 3 O 4 The CuO fiber has a specific structure and is subjected to alkali liquor soaking treatment so as to lead the polyaniline/Fe 3 O 4 The CuO fiber has good adsorption performance on halogen ions.
The invention provides polyaniline/Fe 3 O 4 CuO fiber, polyaniline/Fe 3 O 4 The CuO fibers are interlaced with each other to form clusters having a cage-like structure.
Preferably, polyaniline/Fe 3 O 4 The diameter of the CuO fiber is less than or equal to 200nm.
The invention also provides the polyaniline/Fe 3 O 4 The preparation method of the CuO fiber comprises the following steps: nano Fe 3 O 4 Mixing nano CuO and aniline, soaking, adding protonic acid water solution, mixing, regulating temperature, and dripping initiator water solutionThermal insulation reaction, solid-liquid separation to obtain polyaniline/Fe 3 O 4 CuO fiber.
Preferably, nano Fe 3 O 4 The weight ratio of the nano CuO to the aniline is 0.5-1:0.5-1:10.
Preferably, the temperature is regulated to be between-10 and 10 ℃, and the reaction time is kept for 8 to 12 hours.
Preferably, the protonic acid is at least one of hydrochloric acid, p-toluenesulfonic acid, nitric acid and sulfuric acid.
Preferably, the concentration of the aqueous solution of protic acid is between 0.25 and 0.35mol/l.
Preferably, the initiator is at least one of ammonium persulfate and sodium persulfate.
Preferably, the concentration of the aqueous initiator solution is from 1.5 to 2mol/L.
Preferably, the volume ratio of the aqueous solution of protonic acid to the aqueous solution of initiator is 15-20:5.
Preferably, the weight to volume ratio of the aniline and the aqueous solution of protonic acid is 1g to 15-20ml.
The invention also provides the polyaniline/Fe 3 O 4 Use of CuO fibers for adsorbing halogen ions.
Preferably, polyaniline/Fe 3 O 4 After soaking CuO fiber in alkaline solution, halogen ion is adsorbed in the environment with pH less than 10.
The invention uses polyaniline/Fe 3 O 4 The CuO fiber is treated by alkali liquor, so that the CuO fiber has a large amount of active amino and imino, has good adsorption performance, and is polyaniline/Fe 3 O 4 The CuO fibers are mutually staggered to form clusters with cage structures, the structures can be mutually matched with active amino groups, and meanwhile, the electrostatic attraction effect is combined, so that halogen ions are adsorbed and fixed, and the adsorption performance is improved.
Preferably, the halogen ions are adsorbed in an environment with a pH of not less than 10.
Preferably, polyaniline/Fe 3 O 4 The amount of CuO fiber is 1-10g, and the concentration of halogen ion in the solution to be adsorbed is 1000-15000g/L.
Preferably, the adsorption time is 1-15min and the adsorption temperature is 10-30 ℃.
Preferably, the soaking is carried out for 1-30min.
Preferably, the alkaline solution is at least one of an aqueous sodium hydroxide solution and an aqueous potassium hydroxide solution.
Preferably, the mass fraction of the aqueous sodium hydroxide solution is 8-39wt%.
The inventors selected the appropriate pH, polyaniline/Fe 3 O 4 CuO fiber amount and halogen ion concentration, etc., so that polyaniline/Fe 3 O 4 The CuO fiber has good adsorption performance on halogen ions.
The beneficial effects are that:
the invention selects a proper method to prepare polyaniline/Fe 3 O 4 CuO fiber, polyaniline/Fe 3 O 4 The CuO fibers are mutually staggered to form clusters with cage-shaped structures, so that the invention has specific morphology and polyaniline/Fe 3 O 4 The CuO fiber is treated by alkali liquor, so that the CuO fiber has a large amount of active amino and imino, has good adsorption performance, and is polyaniline/Fe 3 O 4 The CuO fibers are mutually staggered to form clusters with cage-shaped structures, the structures can be mutually matched with active amino groups, and simultaneously the electrostatic attraction effect is combined to achieve the effect of adsorbing and fixing halogen ions, so that polyaniline/Fe 3 O 4 CuO fiber has good adsorption performance on halogen ions; and polyaniline/Fe 3 O 4 The CuO fiber is easy to recycle and can be reused.
Drawings
FIG. 1 shows polyaniline/Fe obtained in example 1 3 O 4 Electron microscope pictures of CuO fibers.
Detailed Description
The technical scheme of the present invention will be described in detail by means of specific examples, which should be explicitly set forth for illustration, but should not be construed as limiting the scope of the present invention.
Example 1
polyaniline/Fe 3 O 4 Process for preparing CuO fibers, comprising, for exampleThe method comprises the following steps: 1g of nano Fe 3 O 4 Mixing 1g of nano CuO with 10ml of aniline, soaking, adding 170ml of 0.3mol/l p-toluenesulfonic acid aqueous solution, mixing, regulating the temperature to 0 ℃, dripping 50ml of 2mol/l initiator aqueous solution, reacting for 10 hours at the temperature to obtain a dark green solution, centrifuging, taking precipitate, respectively washing the precipitate with ethanol and water for three times, and drying to obtain polyaniline/Fe 3 O 4 CuO fiber.
For the polyaniline/Fe 3 O 4 The results of the detection of CuO fiber are shown in FIG. 1, FIG. 1 shows polyaniline/Fe prepared in example 1 3 O 4 Electron microscope pictures of CuO fibers.
As can be seen from fig. 1: polyaniline/Fe 3 O 4 The CuO fibers are mutually staggered to form clusters with cage-shaped structures, and polyaniline/Fe 3 O 4 The diameter of the CuO fiber is less than or equal to 200nm.
Example 2
polyaniline/Fe 3 O 4 The preparation method of the CuO fiber comprises the following steps: 0.5g of nano Fe 3 O 4 Mixing 1g of nano CuO with 10ml of aniline, soaking, adding 200ml of 0.25mol/l hydrochloric acid aqueous solution, mixing, regulating the temperature to-10 ℃, dropwise adding 50ml of 1.8mol/l initiator aqueous solution, reacting for 12 hours at the temperature to obtain a dark green solution, centrifuging, taking precipitate, respectively washing the precipitate with ethanol and water for three times, and drying to obtain polyaniline/Fe 3 O 4 CuO fiber.
Example 3
polyaniline/Fe 3 O 4 The preparation method of the CuO fiber comprises the following steps: 1g of nano Fe 3 O 4 Mixing 0.5g nano CuO with 10ml aniline, soaking, adding 150ml sulfuric acid water solution of 0.35mol/l, mixing, adjusting the temperature to 10 ℃, dripping 50ml initiator water solution of 1.5mol/l, reacting for 12 hours at the temperature to obtain dark green solution, centrifuging, taking precipitate, washing the precipitate with ethanol and water for three times respectively, and drying to obtain polyaniline/Fe 3 O 4 CuO fiber.
Example 4
The polyaniline/Fe prepared in example 1 was taken 3 O 4 CuO fiber, for examining adsorbentThe effect of the amount and adsorption time on the adsorption amount and adsorption rate was measured in three parallel for each experiment, and the results are shown in tables 1 to 3.
The specific method for adsorbing the bromide ions comprises the following steps: the polyaniline/Fe prepared in example 1 was taken 3 O 4 Soaking CuO fiber in 10wt% concentration sodium hydroxide solution for 10min, washing, adding into pH 8-containing water solution, stirring at 25deg.C for adsorption, filtering, detecting the concentration of bromide ion in the filtrate, and calculating polyaniline/Fe 3 O 4 The adsorption quantity and the removal rate of the CuO fiber to bromide ions.
Adsorption amount= (starting concentration of bromide-concentration after bromide adsorption) ×solution volume/adsorbent mass.
The removal rate = (starting concentration of bromide-concentration after bromide adsorption)/starting concentration of bromide × 100%.
TABLE 1 polyaniline/Fe 3 O 4 Influence of CuO fiber amount on the amount of bromine ion adsorption (adsorption time is 10 min)
As can be seen from Table 1, with polyaniline/Fe 3 O 4 The amount of CuO fiber was increased, the amount of adsorption of bromide ion was gradually increased, and when the amount was 2g, polyaniline/Fe 3 O 4 The adsorption quantity of the CuO fiber to the bromide ion reaches the maximum.
TABLE 2 influence of adsorption time on the amount of bromide ion adsorption (the amount of adsorbent used was 2 g)
As can be seen from table 2: with the increase of adsorption time, the adsorption amount of bromide ions is gradually increasedAnd gradually increases. When polyaniline/Fe 3 O 4 And when the CuO fiber is adsorbed for 10min, the adsorption quantity of the bromide ions is maximum.
TABLE 3 polyaniline/Fe 3 O 4 Influence of CuO fiber amount on the adsorption rate of bromine ions (adsorption time is 10 min)
As can be seen from table 3: with polyaniline/Fe 3 O 4 The adsorption rate is gradually increased when the amount of CuO fiber is increased, and the adsorption rate is increased when the polyaniline/Fe 3 O 4 When the amount of the CuO fiber is 3g, the adsorption rate of bromide ions reaches the maximum, and then the amount of the adsorbent is increased, the adsorption rate is not increased any more, and the average adsorption rate is as high as 98.7%.
Example 5
The polyaniline/Fe prepared in example 1 was taken 3 O 4 The effect of the amount of the adsorbent on the adsorption rate of iodine ions was examined, and three parallel samples were prepared, and the results are shown in Table 4.
polyaniline/Fe 3 O 4 The method for absorbing iodine ions by the CuO fiber comprises the following steps: the polyaniline/Fe prepared in example 1 was taken 3 O 4 And (3) adding CuO fiber into a 10wt% sodium hydroxide aqueous solution for soaking for 30min, washing, adding into an aqueous solution containing iodide ions with pH of 7.5, stirring and adsorbing for 10min at 25 ℃, detecting the concentration of the iodide ions in the filtrate, and calculating the removal rate of the iodide ions.
TABLE 4 polyaniline/Fe 3 O 4 Effect of CuO fiber amount on iodine ion adsorption Rate
As can be seen from table 4: with polyaniline/Fe 3 O 4 The adsorption rate of iodine ions is gradually increased when the consumption of CuO fiber is increased, and when polyaniline/Fe 3 O 4 When the amount of the CuO fiber is 3g, the adsorption rate of iodine ions reaches the maximum, and then the amount of the adsorbent is increased, the adsorption rate is not increased any more, and the average adsorption rate is as high as 99.7%.
Example 6
The polyaniline/Fe prepared in example 1 was taken 3 O 4 The effect of the amount of the adsorbent on the adsorption rate of fluorine ions was examined, and three parallel samples were prepared, and the results are shown in Table 5.
polyaniline/Fe 3 O 4 The method for adsorbing fluoride ions by CuO fiber comprises the following steps: the polyaniline/Fe prepared in example 1 was taken 3 O 4 And (3) adding CuO fiber into a 10wt% sodium hydroxide aqueous solution for soaking for 30min, washing, adding into a fluorine ion-containing aqueous solution with pH of 8.5, stirring and adsorbing for 15min at 20 ℃, detecting the concentration of iodine ions in the filtrate, and calculating the removal rate of the iodine ions.
TABLE 5 polyaniline/Fe 3 O 4 Effect of CuO fiber amount on the fluoride ion adsorption Rate
As can be seen from table 5: with polyaniline/Fe 3 O 4 The adsorption rate of fluorine ions is gradually increased when the consumption of CuO fiber is increased, and when polyaniline/Fe 3 O 4 When the amount of CuO fiber is 3g, the adsorption rate of fluorine ions reaches the maximum, and then the adsorption rate is not increased any more and the average adsorption rate is increased after the amount of the adsorbent is increasedThe attachment rate is as high as 92.1 percent.
Example 7
polyaniline/Fe 3 O 4 The method for adsorbing chloride ions by CuO fiber comprises the following steps: the polyaniline/Fe prepared in example 1 was taken 3 O 4 5g of CuO fiber, adding into 10wt% sodium hydroxide aqueous solution for soaking for 16min, then washing, adding into aqueous solution with pH=8 and containing chloride ions, stirring and adsorbing for 30min at 28 ℃, filtering, detecting the concentration of the chloride ions in the filtrate, and calculating the removal rate of the chloride ions to be 99.6%.
The polyaniline/Fe 3 O 4 After the CuO fiber adsorbs halogen ions to reach saturation, alkali liquor can be used for soaking and removing the halogen ions attached to the adsorbent, and after repeated water washing, the polyaniline/Fe 3 O 4 CuO fibers are repeatedly used for adsorbing halogen ions.
Comparative example 1
Polyaniline material without adding Fe 3 O 4 And CuO, otherwise as in example 1.
Comparative example 2
polyaniline/Fe 3 O 4 The material was the same as in example 1 except that CuO was not added.
Comparative example 3
polyaniline/CuO material without adding Fe 3 O 4 Otherwise, the same as in example 1 was conducted.
Comparative example 4
Polyaniline particles commercially available.
Comparative examples 1 to 4 were taken, and bromide ion, iodide ion, fluoride ion and chloride ion were adsorbed respectively in the same manner as in examples 4 to 7, and the removal rate of each halide ion by polyaniline particles was examined, and the results are shown in Table 6.
TABLE 6 results of halogen ion removal rates for comparative examples 1 to 4
| Removal rate (%) | Comparative example 1 | Comparative example 2 | Comparative example 3 | Comparative example 4 |
| Bromide ion | 10.2 | 11.1 | 9.9 | 10.8 |
| Iodide ion | 16.6 | 17.5 | 15.8 | 16.9 |
| Fluoride ions | 13.3 | 14.8 | 12.7 | 13.8 |
| Chloride ions | 7.3 | 8.9 | 6.9 | 7.9 |
As can be seen from Table 6, polyaniline/Fe 3 O 4 The removal rate of halogen ions by the CuO fiber is good.
Comparative example 5
The polyaniline/Fe prepared in example 1 was taken 3 O 4 CuO fiber is directly added into a halogen ion aqueous solution for adsorption without being soaked in a sodium hydroxide aqueous solution, and the adsorption conditions are the same as those of examples 4-7; the removal rate of each halogen ion was examined, and the results are shown in table 7.
TABLE 7 removal rate results
| Halogen ion | Removal rate (%) |
| Bromide ion | 60.6 |
| Iodide ion | 69.9 |
| Fluoride ions | 56.3 |
| Chloride ions | 33.1 |
As can be seen from Table 7, polyaniline/Fe without alkali liquor soaking 3 O 4 The removal rate of halogen ions of the CuO fiber is lower than that of polyaniline/Fe which is soaked in alkali liquor 3 O 4 CuO fiber, the polyaniline/Fe can be improved by the soaking treatment of alkali liquor 3 O 4 CuO fiber adsorption performance for halogen ions.
The foregoing is only a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art, who is within the scope of the present invention, should make equivalent substitutions or modifications according to the technical scheme of the present invention and the inventive concept thereof, and should be covered by the scope of the present invention.
Claims (5)
1. polyaniline/Fe 3 O 4 The use of CuO fiber for adsorbing halogen ions, characterized in that polyaniline/Fe 3 O 4 After soaking CuO fiber in alkaline solution, adsorbing halogen ions in an environment with pH less than 10;
polyaniline/Fe 3 O 4 The consumption of the CuO fiber is 1-10g, and the concentration of halogen ions in the solution to be adsorbed is 1000-15000g/L; the adsorption time is 1-15min, and the adsorption temperature is 10-30 ℃;
the polyaniline/Fe 3 O 4 CuO fibers are interlaced with each other to form clusters with a cage-like structure;
the polyaniline/Fe 3 O 4 The preparation method of the CuO fiber comprises the following steps: nano Fe 3 O 4 Mixing nano CuO with aniline, soaking, adding protonic acid aqueous solution, mixing, regulating temperature, dripping initiator aqueous solution, maintaining the temperature for reaction, and separating solid from liquid to obtain polyaniline/Fe 3 O 4 CuO fiber;
nano Fe 3 O 4 The weight ratio of the nano CuO to the aniline is 0.5-1:0.5-1:10;
the concentration of the protonic acid aqueous solution is 0.25-0.35mol/L;
the concentration of the initiator aqueous solution is 1.5-2mol/L;
the volume ratio of the protonic acid aqueous solution to the initiator aqueous solution is 15-20:5;
the weight volume ratio of the aniline to the protonic acid aqueous solution is 1g:15-20mL.
2. The polyaniline/Fe according to claim 1 3 O 4 The use of CuO fiber for adsorbing halogen ions, characterized in that polyaniline/Fe 3 O 4 The diameter of the CuO fiber is less than or equal to 200nm.
3. Root of Chinese characterThe polyaniline/Fe according to claim 1 or 2 3 O 4 The application of CuO fiber in adsorbing halogen ion is characterized in that the temperature is regulated to be-10 to 10 ℃, and the reaction time is kept for 8 to 12 hours.
4. The polyaniline/Fe according to claim 1 or 2 3 O 4 The application of the CuO fiber in adsorbing halogen ions is characterized in that the protonic acid is at least one of hydrochloric acid, p-toluenesulfonic acid, nitric acid and sulfuric acid.
5. The polyaniline/Fe according to claim 1 or 2 3 O 4 The application of the CuO fiber in adsorbing halogen ions is characterized in that the initiator is at least one of ammonium persulfate and sodium persulfate.
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