CN103586083A - Preparation method of nonhomogeneous Fenton reagent - Google Patents
Preparation method of nonhomogeneous Fenton reagent Download PDFInfo
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- CN103586083A CN103586083A CN201310467357.6A CN201310467357A CN103586083A CN 103586083 A CN103586083 A CN 103586083A CN 201310467357 A CN201310467357 A CN 201310467357A CN 103586083 A CN103586083 A CN 103586083A
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Abstract
The invention discloses a preparation method of a nonhomogeneous Fenton reagent, which comprises the following steps: a. putting carrier fibers in a metal salt solution, and treating in a 40-90 DEG C water bath; b. adding alkali to regulate the pH value to an alkaline state to generate oxyhydroxide, washing and carrying out vacuum filtration; and c. putting the filtered solid in a drying oven, heating for 2-12 hours, and cooling to room temperature to obtain the nonhomogeneous Fenton reagent. The prepared Fenton reagent can be directly used in a dye solution photodegradation experiment, and successfully solves the problems of high addition amount, difficulty in recovery and separation, loss of active components and severe secondary pollution in the traditional Fenton reagent. The method is applicable to large-scale production and has wide application prospects.
Description
technical field:
The invention belongs to composite preparing technical field, particularly a kind of preparation method of heterogeneous Fenton reagent.
background technology:
Fenton reaction is as a kind of senior chemical oxidation technology, and essence is to use Fe
2+and H
2o
2the Fenton reagent forming, the HO with strong oxidizing property producing by reaction carrys out the organic matter in oxidative degradation waste water.Because can process efficiently various high concentrations, the organic wastewater of difficult degradation, becomes ambient water and processes more and more important method.But traditional homogeneous phase Fenton method has inevitable shortcoming: the first, reagent input amount is large, not complete reaction Fe
2+after reaction finishes, form iron mud, not only wasted a large amount of chemicals and also after reaction finishes, formed secondary pollution; The second, reaction needed is carried out under acid condition, and not only having increased reaction process also has certain corrosion to consersion unit; The 3rd, catalyst recovery difficulty under homogeneous phase Fenton method.In order to overcome these shortcomings, prior art improves traditional Fenton method, most study is on the basis of homogeneous phase Fenton method at present, utilize the immobilization of the principle of physical absorption to active component, but in reaction, still need by adding acid for adjusting pH, just can make reaction system have larger degradation effect, serious to equipment corrosion, secondary pollution is serious.Especially catalytic active component losing issue still exists.
summary of the invention:
The present invention is run off and acid liquid corrosion equipment in order to solve catalytic active component, proposes targetedly a kind of preparation method of heterogeneous Fenton reagent.The carrier fibre with coordination function is immersed in metal salt solution, utilizes coordination precipitation method that metal oxide is deposited on to fiber surface and form heterogeneous Fenton reagent.This preparation method is simple, is applicable to large-scale production.
The preparation method of a kind of heterogeneous Fenton reagent provided by the invention, comprises the following steps:
Step 3, the solid leaching is placed in baking oven and heats 2-12 h, be cooled to room temperature, obtain metal oxide supported fiber, i.e. heterogeneous Fenton reagent.
Described carrier fibre is the acrylic fibers chelate fibre with strong coordination ability.
Described metal salt solution is to contain Fe
3+, Cu
2+in the concentration of any one metal ion configuration be the aqueous solution of 0.05-0.11 mol/L.
Described alkali lye can be NaOH, potassium hydroxide, any one in ammoniacal liquor.
Described metal hydroxides is iron hydroxide, any one of Kocide SD.
Described metal oxide is iron oxide, any one of cupric oxide.
Acrylic fibers chelate fibre loads on fiber surface by the nano-metal-oxide with catalysis.The catalyst of nanostructured shows larger catalytic activity because have compared with large specific area; Be combined with carrier fibre coordination mode, in conjunction with firmly, effectively avoid catalyst to run off with water body, also convenient recycling.Utilization has the acrylic fibers chelate fibre of coordination function as carrier, cheap and easy to get, and stable in properties is nontoxic, can be repeatedly used, and saves the energy, does not produce secondary pollution.
Light-Fenton catalytic degradation experiment by the heterogeneous Fenton reagent of preparing for dyestuff, concrete steps: in light-catalyzed reaction instrument, the heterogeneous Fenton reagent preparing is joined to dyestuff and H
2o
2mixed solution in, carry out photo-Fenton reaction, the change calculations degradation rate of absorbance by dyestuff before and after reaction relatively judges the activity of catalyst and the palliating degradation degree of dyestuff.
Heterogeneous Fenton reagent prepared by this method, active red to 50 mg/L, active yellow, three kinds of dyestuffs of methyl orange carry out photocatalytic degradation research and show, in the situation that not needing acid solution to regulate pH, under neutrallty condition, can react, operate simpler, corrosivity to equipment reduces, and can reach more than 98% to the degradation rate of three kinds of water-soluble dyes; Heterogeneous Fenton just can be realized the recovery problem of catalyst by simple filtration, can repetitive cycling use repeatedly, effectively prevent the losing issue of catalyst activity component, realized the green high-efficient degraded to dye solution under low temperature (10-25 ℃) normal pressure.This technological invention provides a kind of new reference for low-cost degradation of dye waste water.
accompanying drawing explanation:
Fig. 1 Fe
3+the affect figure of concentration on catalyst activity;
The affect figure of Fig. 2 bath temperature on catalyst activity;
The affect figure of Fig. 3 drying time on catalyst activity;
Fig. 4 Fe
2o
3the degradation effect figure of/acrylic fibers chelate fibre to active red dye;
Fig. 5 Fe
2o
3the reusability of/acrylic fibers chelate fibre catalyst;
Fig. 6 Fe
2o
3the general applicability of/acrylic fibers chelate fibre catalyst;
The degradation effect figure of Fig. 7 CuO/ acrylic fibers chelate fibre to active red dye;
The electromicroscopic photograph of Fig. 8 heterogeneous Fenton reagent: (a) Fe
2o
3/ acrylic fibers chelate fibre, (b) CuO/ acrylic fibers chelate fibre;
Heterogeneous light-the Fenton of Fig. 9 catalytic degradation dyewood intention.
Specific embodiments
Embodiment 1: heterogeneous Fenton reagent---Fe
2o
3the preparation of/acrylic fibers chelate fibre
0.50 g carrier fibre is placed in to the Fe of 50 mL
3+in solution, under 70 ℃ of water-baths, complexation reaction 3 h, obtain Fe
3+-acrylic fibers chelate fibre; Add alkali lye to regulate pH to alkalescence, generate Fe (OH)
3/ acrylic fibers chelate fibre; Washing, suction filtration, is placed in the solid leaching in baking oven and adds thermal decomposition, is cooled to room temperature, obtains Fe
2o
3/ acrylic fibers chelate fibre catalyst.
The Fe of research variable concentrations
3+the impact of the catalytic activity of the Fenton reagent of preparing.Keep other preparation conditions constant, regulate Fe
3+the catalyst prepared from 0.05 mol/L ~ 0.11 mol/L of concentration range active red dye is carried out to the experiment of light Fenton catalytic degradation, calculate degradation rate result as shown in Figure 1.As seen from the figure, by the Fe of 0.10 mol/L
3+the Fenton reagent photocatalysis effect that solution is prepared is best, and activity is the highest.
Embodiment 2: heterogeneous Fenton reagent---Fe
2o
3the preparation of/acrylic fibers chelate fibre
As embodiment 1, difference is that bath temperature scope is from 40-90 ℃.After light-catalyzed reaction, calculate degradation rate result as shown in Figure 2.As seen from the figure, the Fenton reagent photocatalysis effect of preparing at 70 ℃ is best, and activity is the highest.
Embodiment 3: heterogeneous Fenton reagent---Fe
2o
3the preparation of/acrylic fibers chelate fibre
As embodiment 1, difference is that drying time scope is from 2-12 h.After light-catalyzed reaction, calculate degradation rate result as shown in Figure 3.As seen from the figure, the Fenton reagent photocatalysis effect of preparing under 6 h is best, and activity is the highest.
Embodiment 4:Fe
2o
3the degradation experiment of/acrylic fibers chelate fibre to active red dye
Configuration concentration is the active red dye solution of 50 mg/L, at maximum absorption wavelength (λ
max=530 nm) locate, recording absorbance is A
0, get 30 mL dye solutions and add hydrogen peroxide and 0.03 gFe
2o
3/ acrylic fibers chelate fibre catalyst after mixing, carries out in light-catalyzed reaction instrument, and light source is the Xe lamp of 300 W.Carry out control experiment simultaneously.Every 20 min, in the maximum absorption wave strong point of solution, measure absorbance A
t, calculate degradation rate D, the computing formula D=(1-A of degradation rate
t/ A
0) * 100%.By degradation rate over time relation list in Fig. 4.The degradation rate of active red dye when 100 min just can approach 100% as seen from the figure.
Embodiment 5:Fe
2o
3the reusability of/acrylic fibers chelate fibre
Prepare one group of dye strength and the identical mixed solution of hydrogen peroxide content, add 0.03 g Fe
2o
3/ acrylic fibers chelate fibre catalyst carries out light-catalyzed reaction.After reaction finishes, isolated by filtration is also used distilled water washing catalyst, for reaction next time.Experimental result is shown in Fig. 5, as seen from the figure, when catalyst is reused the 7th time, the degradation rate of dyestuff is still more than 80%, illustrate that the heterogeneous Fenton reagent a process for preparing has successfully solved the losing issue of catalytic active component, can be realized and being repeatedly used by simple filtration.
Embodiment 6:Fe
2o
3the general applicability of/acrylic fibers chelate fibre
By 0.03 g Fe
2o
3/ acrylic fibers chelate fibre catalyst is respectively used to degrading activity Huang, active red and methyl orange dye solution, and experimental result is as shown in Figure 6.As seen from the figure, the catalyst a process for preparing is to active yellow, and three kinds of water-soluble dyes of active red and methyl orange can be realized 100% degraded, illustrates that the heterogeneous Fenton reagent a process for preparing has high catalytic activity.
Embodiment 7: heterogeneous Fenton reagent---the preparation of CuO/ acrylic fibers chelate fibre
0.50 g carrier fibre is placed in to the Cu of 50 mL 0.10 mol/L
2+in solution, under 50 ℃ of water-baths, complexation reaction 2 h, obtain Cu
2+-acrylic fibers chelate fibre; Add alkali lye to regulate pH to alkalescence, generate Cu (OH)
2/ acrylic fibers chelate fibre; Washing, suction filtration, is placed in 4 h heating in baking oven by the solid leaching, and is cooled to room temperature, obtains CuO/ acrylic fibers chelate fibre catalyst.
The degradation experiment of embodiment 8:CuO/ acrylic fibers chelate fibre to active red dye
As embodiment 4, difference is that catalyst is CuO/ acrylic fibers chelate fibres, by degradation rate over time relation list in Fig. 7.The degradation rate of active red dye when 120 min just can approach 100% as seen from the figure.
Claims (6)
1. a preparation method for heterogeneous Fenton reagent, is characterized in that, the method comprises the following steps:
Step 1, carrier fibre is placed in to metal salt solution 40-90 ℃ water-bath, obtains metal ion carrying fiber;
Step 2, add alkali lye to regulate pH to alkalescence, generate hydroxide, washing, suction filtration, obtains metal hydroxides carrying fiber;
Step 3, the solid leaching is placed in baking oven and heats 2-12 h, be cooled to room temperature, obtain metal oxide supported fiber, i.e. heterogeneous Fenton reagent.
2. the preparation method who states according to step 1 in claim 1, is characterized in that: described carrier fibre is the acrylic fibers chelate fibre with strong coordination ability.
3. according to the preparation method described in step 1 in claim 1, it is characterized in that: described metal salt solution is to contain Fe
3+, Cu
2+in the concentration of any one metal ion configuration be the aqueous solution of 0.05-0.11 mol/L.
4. according to the preparation method described in step 2 in claim 1, it is characterized in that: described alkali lye can be NaOH, potassium hydroxide, any one in ammoniacal liquor.
5. according to the preparation method described in step 2 in claim 1, it is characterized in that: described metal hydroxides is iron hydroxide, any one of Kocide SD.
6. according to the preparation method described in step 3 in claim 1, it is characterized in that: described metal oxide is iron oxide, any one of cupric oxide.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105312055A (en) * | 2015-11-26 | 2016-02-10 | 江苏大学 | Preparation method and application of Fenton-like catalyst |
| CN106552627A (en) * | 2016-11-10 | 2017-04-05 | 浙江理工大学 | A kind of preparation method and applications based on cupric oxide modified carbon fiber |
| CN107983351A (en) * | 2017-11-27 | 2018-05-04 | 中国地质大学（武汉） | A kind of iron/copper bi-metal oxide and preparation method thereof |
| CN108855148A (en) * | 2018-06-15 | 2018-11-23 | 宁夏宝塔化工中心实验室(有限公司) | A kind of preparation method of compound soil type acidic catalyst |
| CN109158105A (en) * | 2018-09-16 | 2019-01-08 | 天津大学 | Core-shell structure Fe3O4@Cu(OH)xThe synthetic method of magnetic nanoparticle |
| CN110227463A (en) * | 2019-05-31 | 2019-09-13 | 浙江工业大学 | A kind of novel fenton catalyst and preparation method thereof for degradable organic pollutant waste water |
| CN112675910A (en) * | 2021-01-11 | 2021-04-20 | 燕山大学 | Amyloid fiber ferric hydroxide heterogeneous Fenton catalyst and preparation method and application thereof |
| CN113499789A (en) * | 2021-04-09 | 2021-10-15 | 黑龙江大学 | Preparation method of tungsten disulfide/Naberlite heterogeneous Fenton-like catalyst |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105312055A (en) * | 2015-11-26 | 2016-02-10 | 江苏大学 | Preparation method and application of Fenton-like catalyst |
| CN106552627A (en) * | 2016-11-10 | 2017-04-05 | 浙江理工大学 | A kind of preparation method and applications based on cupric oxide modified carbon fiber |
| CN106552627B (en) * | 2016-11-10 | 2019-04-23 | 浙江理工大学 | A kind of preparation method and applications based on copper oxide modified carbon fiber |
| CN107983351A (en) * | 2017-11-27 | 2018-05-04 | 中国地质大学（武汉） | A kind of iron/copper bi-metal oxide and preparation method thereof |
| CN108855148A (en) * | 2018-06-15 | 2018-11-23 | 宁夏宝塔化工中心实验室(有限公司) | A kind of preparation method of compound soil type acidic catalyst |
| CN109158105A (en) * | 2018-09-16 | 2019-01-08 | 天津大学 | Core-shell structure Fe3O4@Cu(OH)xThe synthetic method of magnetic nanoparticle |
| CN110227463A (en) * | 2019-05-31 | 2019-09-13 | 浙江工业大学 | A kind of novel fenton catalyst and preparation method thereof for degradable organic pollutant waste water |
| CN112675910A (en) * | 2021-01-11 | 2021-04-20 | 燕山大学 | Amyloid fiber ferric hydroxide heterogeneous Fenton catalyst and preparation method and application thereof |
| CN112675910B (en) * | 2021-01-11 | 2022-03-25 | 燕山大学 | Amyloid fiber ferric hydroxide heterogeneous Fenton catalyst and preparation method and application thereof |
| CN113499789A (en) * | 2021-04-09 | 2021-10-15 | 黑龙江大学 | Preparation method of tungsten disulfide/Naberlite heterogeneous Fenton-like catalyst |
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Application publication date: 20140219 |