CN108636452B - Preparation method and application of chitosan-loaded zero-valent iron pellet catalyst - Google Patents
Preparation method and application of chitosan-loaded zero-valent iron pellet catalyst Download PDFInfo
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- CN108636452B CN108636452B CN201810470825.8A CN201810470825A CN108636452B CN 108636452 B CN108636452 B CN 108636452B CN 201810470825 A CN201810470825 A CN 201810470825A CN 108636452 B CN108636452 B CN 108636452B
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- valent iron
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- persulfate
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 55
- 229920001661 Chitosan Polymers 0.000 title claims abstract description 39
- 239000003054 catalyst Substances 0.000 title claims abstract description 28
- 239000008188 pellet Substances 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 15
- 239000000243 solution Substances 0.000 claims abstract description 15
- JRKICGRDRMAZLK-UHFFFAOYSA-L peroxydisulfate Chemical compound [O-]S(=O)(=O)OOS([O-])(=O)=O JRKICGRDRMAZLK-UHFFFAOYSA-L 0.000 claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 230000007935 neutral effect Effects 0.000 claims abstract description 10
- 239000011259 mixed solution Substances 0.000 claims abstract description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000008367 deionised water Substances 0.000 claims abstract description 8
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 8
- 238000003756 stirring Methods 0.000 claims abstract description 8
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims abstract description 7
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims abstract description 7
- 239000002957 persistent organic pollutant Substances 0.000 claims abstract description 7
- 239000004005 microsphere Substances 0.000 claims abstract description 6
- 239000000843 powder Substances 0.000 claims abstract description 6
- 238000000034 method Methods 0.000 claims abstract description 5
- 239000006228 supernatant Substances 0.000 claims abstract description 4
- 238000005406 washing Methods 0.000 claims abstract description 4
- 239000002351 wastewater Substances 0.000 claims description 9
- 238000011282 treatment Methods 0.000 claims description 6
- LCPVQAHEFVXVKT-UHFFFAOYSA-N 2-(2,4-difluorophenoxy)pyridin-3-amine Chemical group NC1=CC=CN=C1OC1=CC=C(F)C=C1F LCPVQAHEFVXVKT-UHFFFAOYSA-N 0.000 claims description 4
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Substances [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 claims description 4
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 2
- 238000001291 vacuum drying Methods 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 abstract description 6
- 229910021645 metal ion Inorganic materials 0.000 abstract description 6
- 238000001035 drying Methods 0.000 abstract description 4
- 229910052742 iron Inorganic materials 0.000 description 6
- RZVAJINKPMORJF-UHFFFAOYSA-N Acetaminophen Chemical compound CC(=O)NC1=CC=C(O)C=C1 RZVAJINKPMORJF-UHFFFAOYSA-N 0.000 description 4
- 238000002386 leaching Methods 0.000 description 4
- 229960005489 paracetamol Drugs 0.000 description 4
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 230000001590 oxidative effect Effects 0.000 description 3
- 230000015556 catabolic process Effects 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 238000004128 high performance liquid chromatography Methods 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- FHHJDRFHHWUPDG-UHFFFAOYSA-L peroxysulfate(2-) Chemical compound [O-]OS([O-])(=O)=O FHHJDRFHHWUPDG-UHFFFAOYSA-L 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229920002101 Chitin Polymers 0.000 description 1
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical compound [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 description 1
- 230000003213 activating effect Effects 0.000 description 1
- 238000009303 advanced oxidation process reaction Methods 0.000 description 1
- 239000011324 bead Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 230000006196 deacetylation Effects 0.000 description 1
- 238000003381 deacetylation reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000000635 electron micrograph Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 229910001447 ferric ion Inorganic materials 0.000 description 1
- 229910001448 ferrous ion Inorganic materials 0.000 description 1
- 150000004676 glycans Chemical class 0.000 description 1
- 239000002638 heterogeneous catalyst Substances 0.000 description 1
- TUJKJAMUKRIRHC-UHFFFAOYSA-N hydroxyl Chemical compound [OH] TUJKJAMUKRIRHC-UHFFFAOYSA-N 0.000 description 1
- -1 iron ions Chemical class 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000011866 long-term treatment Methods 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 229920001282 polysaccharide Polymers 0.000 description 1
- 239000005017 polysaccharide Substances 0.000 description 1
- 239000010802 sludge Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000002560 therapeutic procedure Methods 0.000 description 1
- 229910001428 transition metal ion Inorganic materials 0.000 description 1
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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
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/02—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides
- B01J31/06—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides containing polymers
-
- B01J35/51—
-
- 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
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/722—Oxidation by peroxides
-
- 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
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
-
- 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
- C02F2101/30—Organic compounds
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/02—Specific form of oxidant
Abstract
The invention discloses a preparation method and application of a chitosan-loaded zero-valent iron pellet catalyst, which comprises the following steps: (1) chitosan and FeCl3·6H2Adding O into deionized water, stirring and dissolving to obtain mixed gel; (2) adding zero-valent iron powder into the mixed gel solution to obtain a mixed solution; (3) dropwise adding the mixed solution into NaOH solution by using an injector to form chitosan loaded zero-valent iron pellets; (4) and (4) washing the chitosan zero-valent iron-loaded pellets prepared in the step (3) with ethanol and deionized water until the supernatant is neutral, and drying in vacuum. The chitosan loaded zero-valent iron microsphere catalyst prepared by the method disclosed by the invention and persulfate act synergistically, external energy is not required, the conditions required by the reaction can be achieved under the normal-temperature neutral pH condition, and compared with a homogeneous persulfate system, the heterogeneous persulfate system can continuously provide sulfate radicals and reduce the release amount of metal ions, so that organic pollutants in water are continuously degraded, and secondary pollution is also prevented.
Description
Technical Field
The invention belongs to the technical field of catalysts, and particularly relates to a preparation method and application of a chitosan-loaded zero-valent iron pellet catalyst.
Background
Advanced oxidation processes have been extensively studied and can be used to remove organic materials that are difficult to biochemically degrade. Fenton and Fenton-like reactions are more applied in a chemical oxidation method, and have the advantage that the generated hydroxyl radicals with strong oxidizing property can effectively oxidize and degrade most organic matters. However, because of its harsh requirements on reaction conditions (pH of about 3.0), H2O2The cost is high, the storage is difficult, and the subsequent biochemical treatment needs to adjust the pH of the inlet water, thereby causing the treatment cost to be overhigh.
Based on sulfate radicals (SO)4 -Persulfate (PS) and Peroxymonosulfate (PMS) are novel advanced oxidation technologies developed in recent years. Because the reaction condition is mild and does not depend on the pH value, the generated sulfate radical has strong oxidizability and longer half-life period than hydroxyl radical, and can continuously oxidize organic matters until the organic matters are mineralized. Transition metal ion (e.g. Fe)2+，Cu2+，Ag+And Co2+) Has been shown to be effective in activating PS. In particular, Fe2+Are often used for therapy. The zero-valent iron and the nano zero-valent iron can more effectively activate PS to degrade pollutants similar to a Fenton system, however, Fe0High Fe in/PS systems2+The concentration of which can lead to SO4 -Thus reducing the efficiency of contaminant degradation. The released iron ions and iron sludge with too high concentration will certainly cause environmental pollution. In addition, ferrous ions are easily oxidized to ferric ions, resulting in a decrease in catalytic activity. In view of long-term treatment, a suitable support matrix may be used instead of pure Fe0Or soluble Fe2+To improve the sustainability of the catalyst. Thus, loading iron species onto solid matrix materials seems promising for the formation of heterogeneous catalysts with considerable effectiveness.
Chitosan (CS) is a linear natural polysaccharide obtained from the deacetylation of chitin, either wholly or partially. In recent years, chitosan has been widely studied and used as a support for iron-based substances due to its low cost, ready availability, environmental friendliness, and excellent ability to bind metal ions.
At present, the use of chitosan-supported cross-linking metal ions as a catalyst for Fenton reaction is studied, but the research on the catalytic effect of persulfate is not yet mature.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a preparation method of a chitosan loaded zero-valent iron pellet catalyst.
The invention also aims to provide application of the chitosan-loaded zero-valent iron pellet catalyst.
The technical scheme of the invention is as follows:
a preparation method of a chitosan-loaded zero-valent iron pellet catalyst comprises the following steps:
(1) chitosan and FeCl3·6H2Adding O into deionized water, stirring and dissolving to obtain mixed gel;
(2) adding zero-valent iron powder into the mixed gel solution obtained in the step (1) and then uniformly stirring to obtain a mixed solution;
(3) dropwise adding the mixed solution obtained in the step (2) into a NaOH solution by using an injector to form chitosan loaded zero-valent iron pellets;
(4) washing the chitosan loaded zero-valent iron pellets prepared in the step (3) with ethanol and deionized water until the supernatant is neutral, and vacuum-drying at 60-65 ℃ for 12-16 h to obtain the chitosan loaded zero-valent iron pellet catalyst.
In a preferred embodiment of the present invention, in the step (1), chitosan and FeCl3·6H2The mass ratio of O is 1: 2-3.
In a preferred embodiment of the present invention, the step (2) is: and (2) adding zero-valent iron powder into the mixed gel solution obtained in the step (1) until the final concentration is 0.04-0.07 mol/L, and uniformly stirring to obtain a mixed solution.
In a preferred embodiment of the present invention, the concentration of the sodium hydroxide solution in the step (3) is 1.0 to 3.0 mol/L.
The chitosan load zero-valent iron pellet catalyst prepared by the preparation method is applied to the treatment of wastewater containing organic pollutants.
In a preferred embodiment of the invention, comprises: under the conditions of normal temperature and neutral pH, the chitosan-loaded zero-valent iron microsphere catalyst and persulfate are added into the wastewater together, the concentration of the persulfate in the wastewater is 1.0-3.0 mM, and the concentration of the chitosan-loaded zero-valent iron microsphere catalyst in the wastewater is 0.8-1.2 g/L.
Further preferably, the persulfate is sodium persulfate and/or potassium persulfate.
The invention has the beneficial effects that:
1. the chitosan load zero-valent iron globule catalyst prepared by the preparation method of the invention is added into the wastewater containing organic pollutants together with persulfate, and the two are contacted to form a large amount of sulfate radicals with strong oxidizing property, thereby oxidizing the organic pollutants to degrade the organic pollutants,
2. the chitosan loaded zero-valent iron microsphere catalyst prepared by the method disclosed by the invention and persulfate act synergistically, external energy is not required, the conditions required by the reaction can be achieved under the normal-temperature neutral pH condition, and compared with a homogeneous persulfate system, the heterogeneous persulfate system can continuously provide sulfate radicals and reduce the release amount of metal ions, so that organic pollutants in water are continuously degraded, and secondary pollution is also prevented.
3. Compared with pure zero-valent iron, the chitosan loaded zero-valent iron bead catalyst prepared by the preparation method can more effectively control metal ion leaching.
Drawings
FIG. 1 is an electron micrograph of a chitosan-supported zero-valent iron pellet catalyst finally obtained in example 1 of the present invention.
Fig. 2 is a diagram of a chitosan-supported zero-valent iron pellet catalyst prepared in example 1 of the present invention (fig. 2(a) is before drying, and fig. 2(b) is after drying).
FIG. 3 is a graph showing the effect of different systems for treating paracetamol in water and the leaching of metal ions in the water according to example 1 of the present invention.
Detailed Description
The technical solution of the present invention will be further illustrated and described below with reference to the accompanying drawings by means of specific embodiments.
Example 1
(1) Chitosan and FeCl3·6H2Adding O into deionized water, stirring and dissolving to obtain mixed gel, chitosan and FeCl3·6H2The mass ratio of O is 1: 2-3;
(2) adding zero-valent iron powder into the mixed gel solution obtained in the step (1) until the final concentration is 0.04-0.07 mol/L, and uniformly stirring to obtain a mixed solution;
(3) dropwise adding the mixed solution obtained in the step (2) into a NaOH solution with the concentration of 1.0-3.0 mol/L by using an injector to form chitosan-loaded zero-valent iron pellets (as shown in figure 2);
(4) washing the chitosan loaded zero-valent iron pellets prepared in the step (3) with ethanol and deionized water until the supernatant is neutral, and drying the chitosan loaded zero-valent iron pellets for 12 to 16 hours at the temperature of 60 to 65 ℃ in vacuum to obtain the chitosan loaded zero-valent iron pellet catalyst shown in the figures 1 and 2
100mL of a solution containing 30mg/L of paracetamol was added to the reactor, and sodium persulfate and chitosan-supported zero-valent iron pellet catalysts were added to the solution so that the concentrations thereof were 3.0mM and 1.2g/L, respectively. The effect of the treatment was examined by high performance liquid chromatography, as shown in FIG. 3, at room temperature and at a neutral pH. The degradation efficiency of the paracetamol after 35min is 98.5 percent, and the total iron leaching amount is 11.3 mg/L.
Comparative example 1
Using the same system, 100mL of a solution containing 30mg/L of paracetamol was added to the reactor, sodium persulfate was added to the solution so that the concentrations thereof were 3.0mM, respectively, and zero-valent iron powder alone was added. The effect of the treatment is detected by high performance liquid chromatography, as shown in figure 3, under the conditions of room temperature and neutral pH value, the total iron leaching amount is 32.3mg/L, which is far larger than that of the catalyst prepared by the invention.
The above description is only a preferred embodiment of the present invention, and therefore should not be taken as limiting the scope of the invention, which is defined by the appended claims.
Claims (4)
1. A preparation method of a chitosan-loaded zero-valent iron pellet catalyst is characterized by comprising the following steps: the method comprises the following steps:
(1) chitosan and FeCl3·6H2Adding O into deionized water, stirring and dissolving to obtain mixed gel, chitosan and FeCl3·6H2The mass ratio of O is 1: 2-3;
(2) adding zero-valent iron powder into the mixed gel solution obtained in the step (1) until the final concentration is 0.04-0.07 mol/L, and uniformly stirring to obtain a mixed solution;
(3) dropwise adding the mixed solution obtained in the step (2) into a NaOH solution with the concentration of 1.0-3.0 mol/L by using an injector to form chitosan-loaded zero-valent iron pellets;
(4) washing the chitosan loaded zero-valent iron pellets prepared in the step (3) with ethanol and deionized water until the supernatant is neutral, and vacuum-drying at 60-65 ℃ for 12-16 h to obtain the chitosan loaded zero-valent iron pellet catalyst.
2. The use of the chitosan-supported zero-valent iron pellet catalyst prepared by the preparation method of claim 1 in the treatment of wastewater containing organic pollutants.
3. Use according to claim 2, characterized in that: the method comprises the following steps: under the conditions of normal temperature and neutral pH, the chitosan-loaded zero-valent iron microsphere catalyst and persulfate are added into the wastewater together, the concentration of the persulfate in the wastewater is 1.0-3.0 mM, and the concentration of the chitosan-loaded zero-valent iron microsphere catalyst in the wastewater is 0.8-1.2 g/L.
4. Use according to claim 3, characterized in that: the persulfate is sodium persulfate and/or potassium persulfate.
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| CN110743549B (en) * | 2019-10-25 | 2022-09-09 | 北京工业大学 | Preparation method of copper-based heterogeneous catalyst taking activated carbon spheres as carrier for wet oxidation |
| CN112316916B (en) * | 2020-11-05 | 2023-07-04 | 重庆交通大学 | Mesoporous core-shell structure nano zero-valent iron gel microsphere for stably loading citrate organic ligand and preparation method thereof |
| CN115367858B (en) * | 2022-08-16 | 2023-11-21 | 华侨大学 | Water treatment method for promoting degradation of paracetamol by monopersulfate heat activation system and cooperatively controlling generation of chlorinated organic byproducts |
| CN116212952A (en) * | 2023-02-20 | 2023-06-06 | 四川大学 | Preparation method and application of tannin chemical derived heterogeneous nano zero-valent iron catalyst |
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| CN103480341A (en) * | 2013-10-14 | 2014-01-01 | 中国科学院城市环境研究所 | Hydrogel material capable of removing arsenic |
| CN105110448A (en) * | 2015-10-09 | 2015-12-02 | 中国科学院南海海洋研究所 | Method for removing heavy metal and organic matter composite pollutants in water body by means of zero-valent iron and persulfate |
| CN105646902A (en) * | 2016-04-01 | 2016-06-08 | 江苏大学 | Preparation method of iron-chitosan metal supermolecular gel |
| CN107445289A (en) * | 2017-08-22 | 2017-12-08 | 西安交通大学 | PVA/ chitosan sphere bio-carriers and preparation method thereof |
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Patent Citations (4)
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| CN103480341A (en) * | 2013-10-14 | 2014-01-01 | 中国科学院城市环境研究所 | Hydrogel material capable of removing arsenic |
| CN105110448A (en) * | 2015-10-09 | 2015-12-02 | 中国科学院南海海洋研究所 | Method for removing heavy metal and organic matter composite pollutants in water body by means of zero-valent iron and persulfate |
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