CN103663631B - Three-dimensional particle electrode loaded with catalyst active carbon and preparation method thereof - Google Patents
Three-dimensional particle electrode loaded with catalyst active carbon and preparation method thereof Download PDFInfo
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- CN103663631B CN103663631B CN201310665223.5A CN201310665223A CN103663631B CN 103663631 B CN103663631 B CN 103663631B CN 201310665223 A CN201310665223 A CN 201310665223A CN 103663631 B CN103663631 B CN 103663631B
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Abstract
The invention discloses a three-dimensional particle electrode loaded with catalyst active carbon and a preparation method thereof. The electrode consists of particle active carbon and a TiO2 solid solution compound catalyst which is loaded on the particle active carbon and is doped with Sn and Sb elements. The method comprises the steps of particle active carbon pretreatment, catalyst preparation, soaking for aging, drying and roasting for activating. The three-dimensional particle electrode loaded with the catalyst active carbon prepared with the method has the characteristics of high pollutant removing rate, high electrocatalytic activity, high yield of hydroxyl radicals, little loss of a catalyst and the like; moreover, the preparation method is simple, noble metal catalysts are not used, used raw materials are widely available, the manufacturing cost is low, and secondary pollution is avoided. When the three-dimensional particle electrode loaded with the catalyst active carbon prepared with the method is applied to a three-dimensional electrode reactor, non-biodegradable organic waste water can be treated efficiently.
Description
Technical field
The present invention relates to three dimensional particles electrode of a kind of supported catalyst gac and preparation method thereof, can be used as 3 D electrode reactor particle filled composite and for difficult for biological degradation treatment of Organic Wastewater, belong to electrochemical catalytic field.
Background technology
In recent years, bipolar three-dimensional electrode reactor is subject to extensive concern.Owing to not arranging barrier material between anode and cathode in the reactor, three dimensional particles electrode is filled between anode and cathode, particle has two kinds of electric polarities under electric field action simultaneously, each three dimensional particles electrode forms micro-electrochemical oxidation system, therefore make multipole reactor be more suitable for irreversible oxidizing reaction, thus there is following characteristics: (1) has that specific surface area is large, face body than large, unit cell body treatment capacity is large; (2) organic pollutant degradation is effective; (3) rate of mass transfer is fast, current efficiency is high, low power consumption and other advantages; (4) be applicable to process the lower waste water of specific conductivity, save and add extra electrolytical expense in two-dimensional electrode uses.Three dimensional particles electrode is the important component part of bipolar three-dimensional electrode reactor; Existing granule electrode is mainly with loading type γ-A1
2o
3, carried molecular sieve, loading type pottery, Coated Activated Carbon, supported catalyst gac be main, but still there is following problem in above granule electrode: (1) loading type γ-A1
2o
3, there is more serious catalyst loss problem in carried molecular sieve, and due to its amphoteric character, resistance to acids and bases is poor, is not therefore suitable for and uses in the alkaline waste water of strongly-acid; (2) loading type ceramic surface is covered by organism and peels off and also causes loss of active component serious, and pottery is expensive due to it simultaneously, to a certain degree limits it and applies; (3) gac has high-specific surface area, cheap and easy to get, chemical stability good and have absorption property concurrently, but load (Mn, Fe, Zn, Ni, CeO
2/ Sb
2o
3, SnO
2/ Sb
2o
3) still to there is catalyst activity not high for gac three dimensional particles electrode, the problems such as catalyst loss, its major cause is that a) catalyzer activity itself is low; B) shortcoming such as catalyst particle size large, poor adhesive force, easily loss.
Summary of the invention
The object of this invention is to provide three dimensional particles electrode of a kind of supported catalyst gac and preparation method thereof, make it have the features such as pollutants removal rate is high, catalytic activity is high, catalyst stream vector is low and preparation method is simple.
Technical scheme of the present invention is as follows:
A three dimensional particles electrode for supported catalyst gac, is characterized in that: by granulated active carbon and load, the composite catalyst on granulated active carbon is formed this granule electrode; Described composite catalyst is the TiO of doping Sn and Sb element
2sosoloid.
In composite catalyst of the present invention, Sn and Ti elemental mole ratios is 0.005 ~ 0.03:1; The mol ratio of Sn and Sb element is 10 ~ 20:1.
The preparation method of the three dimensional particles electrode of a kind of supported catalyst gac provided by the invention, is characterized in that the method comprises the following steps:
1) granulated active carbon pre-treatment: soaked in deionized water by granulated active carbon, after the specific conductivity in mensuration water is consistent with deionized water, is filtered dry excessive moisture and puts into baking oven through 100 DEG C ~ 200 DEG C dryings, being cooled to room temperature stand-by;
2) catalyst preparing: by tetrabutyl titanate and dehydrated alcohol, SnCl
45H
2o and SbCl
3be mixed with solution A; Again deionized water, dehydrated alcohol and acetic acid are configured to B solution; B solution is added drop-wise to slowly in solution A the sol solutions also formed containing Ti, Sn and Sb, in this sol solutions, the mol ratio of Sn and Ti is 0.005 ~ 0.03:1; The mol ratio of Sn and Sb is 10 ~ 20:1;
3) ageing is flooded: be immersed in step 2 by step 1) through pretreated granulated active carbon) the middle sol solutions prepared
In, and carry out ageing formation gel particle;
4) dry oven dry: the gel particle formed in step 3) is placed in vacuum drying oven, at 80 DEG C ~ 95 DEG C dry 8h ~ 24h;
5) calcination activation: dried gel particle is put into retort furnace, fires 2h ~ 3h, naturally cools to room temperature at the temperature of 500 DEG C ~ 550 DEG C, namely obtains the three dimensional particles electrode of supported catalyst gac.
The present invention compared with prior art, has the following advantages and the technique effect of high-lighting: the composite catalyst coating that 1. prepared by the present invention presents the layered distribution (Fig. 1) of nanoscale (median size 10nm), and with stable TiO
2-SnO
2there is (Fig. 3, Fig. 4) in/Sb solid solution thereof, hydroxyl radical free radical generation high (Fig. 2), therefore ensure that loading type three dimensional particles electrode possesses higher structural stability, catalyst stream vector is low and catalytic activity is high feature; 2. the loading type three dimensional particles application of electrode that prepared by the present invention can process difficult for biological degradation organic waste water efficiently, pollutants removal rate high (table 1) in 3 D electrode reactor; 3. preparation method of the present invention is simple, does not use noble metal catalyst, raw materials wide material sources, cheap for manufacturing cost, high without the dirty catalytic activity of secondary.
Accompanying drawing explanation
Fig. 1 is three dimensional particles electrode surface scanning electron microscope (SEM) photograph of the present invention.
Fig. 2 is three dimensional particles electrode hydroxyl radical free radical generation of the present invention.
Fig. 3 is three dimensional particles pole catalyze layer X-ray diffractogram of the present invention.
Fig. 4 is three dimensional particles pole catalyze layer Raman spectrogram of the present invention.
Embodiment
Embodiment 1:
The loading type three dimensional particles electrode of the present embodiment is the TiO of Sn, Sb element of being adulterated on granulated active carbon by granulated active carbon and load
2composite catalyst composition; The TiO of described doping Sn, Sb element
2in composite catalyst, the mol ratio of Sn and Ti is 0.005:1; The mol ratio of Sn and Sb is 10:1.Preparation method comprises the following steps:
1) grain active carbon pre-treatment: soaked by granulated active carbon and clean in deionized water, the specific conductivity measured in rinse water is consistent with deionized water, elimination excessive moisture puts into baking oven 100 DEG C of dryings and to be cooled to room temperature stand-by;
2) catalyst preparing: take 5.7 × 10
-2mol tetrabutyl titanate, 2.85 × 10
-4mol SnCl
45H
2o, 2.85 × 10
-5mol SbCl
3be dissolved in 40mL dehydrated alcohol, rapid stirring 30min, makes solution A.Take 5mL deionized water, 1.5mL acetic acid to be dissolved in 40ml dehydrated alcohol and rapid stirring 30min, makes solution B.B solution is added drop-wise in solution A, solution A vigorous stirring in dropping process, obtains pale yellow transparent and contain Ti, Sn and Sb elemental sols liquid;
3) flood ageing: will be immersed in above-mentioned sol solutions through pretreated granulated active carbon, and carry out ageing formation gel particle;
4) dry oven dry: formation gel particle is placed in vacuum drying oven, at 80 DEG C of dry 24h;
5) calcination activation: just dried gel particle puts into retort furnace, after firing 3h, naturally cools to room temperature at 500 DEG C.
Embodiment 2:
The loading type three dimensional particles electrode of the present embodiment is the TiO of Sn, Sb element of being adulterated on granulated active carbon by granulated active carbon and load
2composite catalyst composition; The TiO of described doping Sn, Sb element
2in composite catalyst, the mol ratio of Sn and Ti is 0.03:1; The mol ratio of Sn and Sb is 20:1.Preparation method comprises the following steps:
1) grain active carbon pre-treatment: soaked by granulated active carbon and clean in deionized water, the specific conductivity measured in rinse water is consistent with deionized water, elimination excessive moisture puts into baking oven 200 DEG C of dryings and to be cooled to room temperature stand-by;
2) catalyst preparing: take 5.7 × 10
-2mol tetrabutyl titanate, 1.71 × 10
-3the SnCl of mol
45H
2o, 8.55 × 10
-5the SbCl of mol
3be dissolved in 40mL dehydrated alcohol, rapid stirring 30min, makes solution A; Take 5mL deionized water, 1.5mL acetic acid to be dissolved in 40ml dehydrated alcohol and rapid stirring 30min, makes solution B.B solution is added drop-wise in solution A, solution A vigorous stirring in dropping process, obtains pale yellow transparent and contain Ti, Sn and Sb elemental sols liquid;
3) flood ageing: will be immersed in above-mentioned sol solutions through pretreated granulated active carbon, and carry out ageing formation gel particle;
4) dry oven dry: formation gel particle is placed in vacuum drying oven, at 95 DEG C of dry 8h;
5) calcination activation: dried gel particle is put into retort furnace, after firing 2h, naturally cools to room temperature at 550 DEG C.
Embodiment 3:
The loading type three dimensional particles electrode of the present embodiment is the TiO of Sn, Sb element of being adulterated on granulated active carbon by granulated active carbon and load
2composite catalyst composition; The TiO of described doping Sn, Sb element
2in composite catalyst, the mol ratio of Sn and Ti is 0.01:1; The mol ratio of Sn and Sb is 10:1.
Preparation method comprises the following steps:
1) grain active carbon pre-treatment: soaked by granulated active carbon and clean in deionized water, the specific conductivity measured in rinse water is consistent with deionized water, elimination excessive moisture puts into baking oven 150 DEG C of dryings and to be cooled to room temperature stand-by;
2) catalyst preparing: take 5.7 × 10
-2mol tetrabutyl titanate, 5.7 × 10
-4mol SnCl
45H
2o, 5.7 × 10
-5mol SbCl
3be dissolved in 40mL dehydrated alcohol, rapid stirring 30min, makes solution A.Take 5mL deionized water, 1.5mL acetic acid to be dissolved in 40ml dehydrated alcohol and rapid stirring 30min, makes solution B.B solution is added drop-wise in solution A, solution A vigorous stirring in dropping process, obtains pale yellow transparent and contain Ti, Sn and Sb elemental sols liquid;
3) flood ageing: will be immersed in above-mentioned sol solutions through pretreated granulated active carbon, and carry out ageing formation gel particle;
4) dry oven dry: formation gel particle is placed in vacuum drying oven, at 90 DEG C of dry 15h;
5) calcination activation: just dried gel particle puts into retort furnace, after firing 2h, naturally cools to room temperature at 500 DEG C.
Embodiment 4:
The loading type three dimensional particles electrode of the present embodiment is the TiO of Sn, Sb element of being adulterated on granulated active carbon by granulated active carbon and load
2composite catalyst composition; The TiO of described doping Sn, Sb element
2in composite catalyst, the mol ratio of Sn and Ti is 0.02:1; The mol ratio of Sn and Sb is 15:1.
Preparation method comprises the following steps:
1) grain active carbon pre-treatment: soaked by granulated active carbon and clean in deionized water, the specific conductivity measured in rinse water is consistent with deionized water, elimination excessive moisture puts into baking oven 150 DEG C of dryings and to be cooled to room temperature stand-by;
2) catalyst preparing: take 5.7 × 10
-2mol tetrabutyl titanate, 1.14 × 10
-4mol SnCl
45H
2o, 7.60 × 10
-5mol SbCl
3be dissolved in 40mL dehydrated alcohol, rapid stirring 30min, makes solution A.Take 5mL deionized water, 1.5mL acetic acid to be dissolved in 40ml dehydrated alcohol and rapid stirring 30min, makes solution B.B solution is added drop-wise in solution A, solution A vigorous stirring in dropping process, obtains pale yellow transparent and contain Ti, Sn and Sb elemental sols liquid;
3) flood ageing: will be immersed in above-mentioned sol solutions through pretreated granulated active carbon, and carry out ageing formation gel particle;
4) dry oven dry: formation gel particle is placed in vacuum drying oven, at 85 DEG C of dry 24h;
5) calcination activation: just dried gel particle puts into retort furnace, after firing 2h, naturally cools to room temperature at 500 DEG C.
Embodiment 5:
The electrolysis effectiveness test of carried active carbon three dimensional particles electrode of the present invention.
The granule electrode prepared in embodiment 1-2 is filled in 3 D electrode reactor and carries out process rhdamine B electrolytic trial (COD:150mg/L, pH=7), wherein ionogen Na
2sO
4concentration is 0.1M, and anode material is titanium base RuO
2-IrO
2-TiO
2-SnO
2coated electrode, negative electrode is stainless steel plate.Preadsorption test is carried out to get rid of adsorbing impact before electrolysis.Test is at continuous current (current density 60mA/cm
2), carry out under hydraulic detention time 3min condition, electrolysis time is 4h, samples and measure COD clearance every half an hour, using the COD average removal rate in 4h as evaluation index.
The three dimensional particles electrode fouling thing removal effect prepared in table 1 embodiment of the present invention
As can be seen from Table 1, the pollutants removal rate of supported catalyst gac three dimensional particles electrode prepared of the present invention is higher than the catalytic efficiency comparing non-loaded particle activated carbon particles.
Embodiment 6: hydroxyl radical free radical determination test
The hydroxyl radical free radical that the supported catalyst three dimensional particles electrolytic process measuring embodiment 1 preparation by electron paramagnetic resonance method (EPR) produces differentiates the electro catalytic activity of three dimensional particles.With the Na of 0.1mol/L
2sO
4solution is electrolytic solution, after the reactor energising 10min of supported catalyst three dimensional particles electrode prepared by filling example 1, add a certain amount of trapping agent DMPO(dimethyl pyridine N-oxide) after to be drawn by EPR method and the spectrogram of OH-EPR characterize the generation of OH by spectrogram medium wave spectral intensity.As Fig. 2 can find out, the hydroxyl radical free radical generation of supported catalyst three dimensional particles electrode prepared by the present invention is about 5 times of non-supported catalyst particle, and illustrate that its electro catalytic activity is high, electrochemical oxidation ability is strong.
Embodiment 7: catalyst loss is tested
The gac three dimensional particles electrode particle in contrast of preparation load Ti element and load Sn and Sb element, by the electrolytic trial that the loading type particle of preparation in embodiment 1 and contrast particle carry out as embodiment 5, by effluent collection and the content measuring wherein catalyzer to characterize the catalyst stream vector of three dimensional particles electrode to evaluate its structural stability.
Table 2 loading type three dimensional particles electrode catalyst wastage
As can be seen from Table 2, the catalyst stream vector of loading type three dimensional particles electrode prepared by the present invention is minimum, the excellent in stability of this three dimensional particles electrode prepared by the present invention is described, mainly because Ti, Sn, Sb form stable sosoloid (Fig. 3, Fig. 4), crystal type and TiO in the Catalytic Layer of supported catalyst gac three dimensional particles electrode prepared of the present invention
2anatase seemingly.
Claims (2)
1. a three dimensional particles electrode for supported catalyst gac, is characterized in that: by granulated active carbon and load, the composite catalyst on granulated active carbon is formed this granule electrode; Described composite catalyst is the TiO of doping Sn and Sb element
2sosoloid; In composite catalyst, the mol ratio of Sn and Ti element is 0.005 ~ 0.03:1; The mol ratio of Sn and Sb element is 10 ~ 20:1.
2. the preparation method of the three dimensional particles electrode of a kind of supported catalyst gac as claimed in claim 1, is characterized in that the method comprises the following steps:
1) granulated active carbon pre-treatment: soaked in deionized water by granulated active carbon, after the specific conductivity in mensuration water is consistent with deionized water, is filtered dry excessive moisture and puts into baking oven through 100 DEG C ~ 200 DEG C dryings, being cooled to room temperature stand-by;
2) catalyst preparing: by tetrabutyl titanate and dehydrated alcohol, SnCl
45H
2o and SbCl
3be mixed with solution A; Again deionized water, dehydrated alcohol and acetic acid are configured to B solution; B solution being added drop-wise to slowly in solution A and forming the sol solutions containing Ti, Sn and Sb, in this sol solutions, the mol ratio of Sn and Ti is the mol ratio of 0.005 ~ 0.03:1, Sn and Sb is 10 ~ 20:1;
3) flood ageing: by step 1) in be immersed in step 2 through pretreated granulated active carbon) in preparation sol solutions in, and carry out ageing formed gel particle;
4) dryly to dry: by step 3) in the gel particle that formed be placed in vacuum drying oven, at 80 DEG C ~ 95 DEG C dry 8h ~ 24h;
5) calcination activation: dried gel particle is put into retort furnace, fires 2h ~ 3h, naturally cools to room temperature at the temperature of 500 DEG C ~ 550 DEG C, namely obtains the three dimensional particles electrode of supported catalyst gac.
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