CN101811755A - Method for preparing sodium dodecyl benzene sulfonate doped titanium catalyzed electrode - Google Patents

Method for preparing sodium dodecyl benzene sulfonate doped titanium catalyzed electrode Download PDF

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CN101811755A
CN101811755A CN200910241595A CN200910241595A CN101811755A CN 101811755 A CN101811755 A CN 101811755A CN 200910241595 A CN200910241595 A CN 200910241595A CN 200910241595 A CN200910241595 A CN 200910241595A CN 101811755 A CN101811755 A CN 101811755A
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electrode
sdbs
ppy
titanium
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CN101811755B (en
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孙治荣
马林
胡翔
彭永臻
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Beijing University of Technology
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Abstract

The invention discloses a method for preparing a sodium dodecyl benzene sulfonate doped titanium catalyzed electrode, belonging to the field of electrochemical water treatment. In the method, a PPy-SDBS/Ti electrode is prepared by electro-deposition by using titanium as an anode, a platinum sheet as a cathode, and pyrrole and sulfuric acid mixed solution added with sodium dodecyl benzene sulfonate as electrolyte, wherein the deposit current density is 0.625mA/cm<2>, and the deposit time is 5 minutes; and the sodium dodecyl benzene sulfonate doped titanium catalyzed electrode is prepared by electro-deposition by using the PPy-SDBS/Ti as a cathode, a platinum sheet as an anode, and PdCl2 solution as electrolyte, wherein the deposit current density is between 2.500 and 5.000mA/cm<2>, and the deposit time is between 25 and 35 minutes. The prepared electrode has obviously improved catalysis activity and low cost, and has certain application prospect.

Description

The preparation method of sodium dodecyl benzene sulfonate-doped titanium catalysis electrode
Technical field
The present invention relates to a kind of preparation method of titanium electrode, relate in particular to that a kind of that have catalytic capability is the preparation method of the adulterated catalysis electrode of Sodium dodecylbenzene sulfonate (SDBS) of matrix with the titanium, be mainly used in electrochemical reduction and remove chlorinatedorganic in the water.
Background technology
The intermediate product that the widespread use of chlorinatedorganic at aspects such as many industry such as chemical industry, medicine, process hides, electronics, agricultural chemicals causes producing in a large amount of chlorine-containing compounds and the building-up process thereof is discharged in the environment.Nearly all chlorinatedorganic is all toxic, and wherein a lot of compounds are considered to have " carcinogenic, teratogenesis, mutagenesis " effect; Simultaneously because a lot of chlorinatedorganics have high volatile volatile and lipoid solubility, easily human body is caused serious harm by absorption such as skin, mucous membrane.Therefore, it is very necessary chlorinatedorganic removal method in the water being studied.For now, the removal method of chlorinatedorganic has burning method, biological degradation method, absorption method, basic metal reduction method and electrochemical techniques etc.Electrochemical process more and more is subject to people's attention aspect environmental pollution improvement as a kind of eco-friendly technology, particularly in waste water aspect the organic removal of bio-refractory.The electrochemical treatment of chlorinatedorganic is meant and remove chlorinatedorganic by electrochemical reaction from sewage, and one of gordian technique of electrochemical reduction dechlorination is electrode under the effect of electrode.In the research of the electrocatalytic hydrogenation dechlorination electrode of being reported in recent years, palladium is because have excellent active hydrogen storage capability, can guarantee that active hydrogen contacts with the chloro organic molecule that is adsorbed continuously and becomes the emphasis of catalyst research.But successively Pd/ activated carbon fiber (Pd/ACF) electrode of report, Pd/GC electrode, Pd/Ti electrode, Pd/Ni electrode etc. are directly with the electrode of metal deposition on base material in recent years, its catalytic activity is general, current efficiency is low when handling the lower concentration chlorinatedorganic, energy consumption is high, can't extensively promote.In addition, there are problems such as resistance is big, unstable properties in the electrode matrix material of some widespread uses, and it is restricted in electrochemical applications.
Summary of the invention
The objective of the invention is to solve the problems of the prior art, and a kind of catalytic activity and current efficiency height are provided, energy consumption is low, the preparation method of the sodium dodecyl benzene sulfonate-doped titanium catalysis electrode of stable performance.
The preparation method of sodium dodecyl benzene sulfonate-doped titanium catalysis electrode provided by the present invention may further comprise the steps:
1) with Palladous chloride (PdCl 2) powder is dissolved in the 3mol/L hydrochloric acid, obtains the PdCl of 20～25mmol/L with the deionized water dilution 2Solution;
2) titanium is embathed 1～3min remove surperficial thing in the sulfuric acid of 0.5mol/L after, again with its successively in acetone (oil removing) and redistilled water respectively ultrasonic oscillation 10～15min clean up dry for standby;
3) pyrroles (Py) was mixed with the sulfuric acid of 0.3mol/L in 7: 1000 by volume, add Sodium dodecylbenzene sulfonate (SDBS) again and obtain mixing solutions, the content of Sodium dodecylbenzene sulfonate is 0.0005～0.002g/mL in the mixing solutions;
4) with step 2) in the oven dry after titanium be anode, platinized platinum is a negative electrode, is electrolytic solution with the mixing solutions of preparing in the step 3), galvanic deposit makes polypyrrole (Sodium dodecylbenzene sulfonate)/titanium electrode (PPy-SDBS/Ti electrode), depositing current density is 0.625mA/cm 2, depositing time is 5min;
5) the PPy-SDBS/Ti electrode that makes with step 4) is a negative electrode, and platinized platinum is an anode, with the PdCl of step 1) preparation 2Solution is electrolytic solution, and galvanic deposit makes sodium dodecyl benzene sulfonate-doped titanium catalysis electrode (Pd/PPy-SDBS/Ti electrode), and depositing current density is 2.500～5.000mA/cm 2, depositing time is 25～35min.
Wherein, the preferred electrodeposition condition in the step 5) is that depositing current density is 2.500mA/cm 2, depositing time is 30min.
Compared with prior art, the present invention has following beneficial effect:
1) the present invention adopts the anionic surfactant sodium dodecylbenzene sulfonate with dispersive ability, prepare sodium dodecyl benzene sulfonate-doped catalysis electrode, the introducing of Sodium dodecylbenzene sulfonate has changed the deposition morphology of pyrroles at electrode surface, and then the deposition form of change Pd on polypyrrole film, thereby increase the specific surface area of electrode, improve its adsorptive power hydrogen atom.
2) the present invention adopts titanium as body material, prepared catalysis electrode stable performance.
3) the present invention adopts the method for electrochemical deposition to prepare the Pd/PPy-SDBS/Ti electrode, has improved the catalytic performance of electrode, and further promoting for it provides possibility.
Description of drawings
Fig. 1 is the cyclic voltammetry curve of the prepared electrode of embodiment 1,2,3.
Fig. 2 is the cyclic voltammetry curve of the prepared electrode of embodiment 4,5 and Comparative Examples.
Among the figure, I is an electric current, E vs Hg/Hg 2SO 4For with respect to Hg/Hg 2SO 4The voltage of reference electrode.
The invention will be further described below in conjunction with the drawings and specific embodiments.
Embodiment
Embodiment 1
1) takes by weighing PdCl 2Powder is dissolved in the 3mol/LHCl solution, adds the PdCl that deionized water is mixed with 22.5mmol/L 2Solution;
2) titanium is embathed 3min remove surperficial thing in 0.5mol/L sulfuric acid after, successively in acetone (oil removing) and redistilled water respectively ultrasonic oscillation 15min clean up dry for standby;
3) with the pyrroles with after the sulfuric acid of 0.3mol/L mixed in 7: 1000 by volume, add Sodium dodecylbenzene sulfonate and obtain mixing solutions, the content of Sodium dodecylbenzene sulfonate is 0.00075g/mL in the mixing solutions;
4) with step 2) in titanium after handling be anode, platinized platinum is a negative electrode, is electrolytic solution with the solution of preparing in the step 3), adopts the method for galvanic deposit to make the PPy-SDBS/Ti electrode, depositing current density is 0.625mA/cm 2, depositing time is 5min;
5) be negative electrode with the PPy-SDBS/Ti electrode, platinized platinum is an anode, with the PdCl for preparing in the step 1) 2Solution is electrolytic solution, and adopting the method for galvanic deposit is 3.125mA/cm in depositing current density 2, depositing time makes the Pd/PPy-SDBS/Ti electrode during for 30min.
The Pd/PPy-SDBS/Ti electrode washing is clean, place 0.5mol/L H 2SO 4In the solution, be counter electrode with the platinized platinum, with Hg/Hg 2SO 4Electrode is that reference electrode carries out cyclic voltammetry scan.The electric potential scanning scope is-700mV～700mV that sweep velocity is 50mV/s.The gained cyclic voltammetry curve is seen a among Fig. 1, the hydrogen adsorption peak occurs about-600mV, and peak point current is-132.56mA.
Embodiment 2
1) takes by weighing PdCl 2Powder is dissolved in the 3mol/L HCl solution, adds the PdCl that deionized water is mixed with 23mmol/L 2Solution;
2) titanium is embathed 2min remove surperficial thing in 0.5mol/L sulfuric acid after, successively respectively in acetone (oil removing) and redistilled water ultrasonic oscillation 12min clean up dry for standby;
3) with the pyrroles with after the sulfuric acid of 0.3mol/L mixed in 7: 1000 by volume, add Sodium dodecylbenzene sulfonate and obtain mixing solutions, the content of Sodium dodecylbenzene sulfonate is 0.001g/mL in the mixing solutions;
4) with step 2) in titanium after handling be anode, platinized platinum is a negative electrode, is electrolytic solution with the solution of preparing in the step 3), adopts the method for galvanic deposit to make the PPy-SDBS/Ti electrode, depositing current density is 0.625mA/cm 2, depositing time is 5min;
5) be negative electrode with the PPy-SDBS/Ti electrode, platinized platinum is an anode, with the PdCl for preparing in the step 1) 2Solution is electrolytic solution, and adopting the method for galvanic deposit is 2.500mA/cm in depositing current density 2, depositing time makes the Pd/PPy-SDBS/Ti electrode during for 30min.
The Pd/PPy-SDBS/Ti electrode washing is clean, place 0.5mol/L H 2SO 4In the solution, be counter electrode with the platinized platinum, with Hg/Hg 2SO 4Electrode is that reference electrode carries out cyclic voltammetry scan.The electric potential scanning scope is-700mV～700mV that sweep velocity is 50mV/s.The gained cyclic voltammetry curve is seen the b among Fig. 1, the hydrogen adsorption peak occurs about-600mV, and peak point current is-137.50mA.
Embodiment 3
1) takes by weighing PdCl 2Powder is dissolved in the 3mol/L HCl solution, adds the PdCl that deionized water is mixed with 24.5mmol/L 2Solution;
2) titanium is embathed 2min remove surperficial thing in 0.5mol/L sulfuric acid after, successively in acetone (oil removing) and redistilled water respectively ultrasonic oscillation 10min clean up dry for standby;
3) with the pyrroles with after the sulfuric acid of 0.3mol/L mixed in 7: 1000 by volume, add Sodium dodecylbenzene sulfonate and obtain mixing solutions, the content of Sodium dodecylbenzene sulfonate is 0.0015g/mL in the mixing solutions;
4) with step 2) in titanium after handling be anode, platinized platinum is a negative electrode, is electrolytic solution with the solution of preparing in the step 3), adopts the method for galvanic deposit to make the PPy-SDBS/Ti electrode, depositing current density is 0.625mA/cm 2, depositing time is 5min;
5) be negative electrode with the PPy-SDBS/Ti electrode, platinized platinum is an anode, with the PdCl for preparing in the step 1) 2Solution is electrolytic solution, and adopting the method for galvanic deposit is 2.500mA/cm in depositing current density 2, depositing time makes the Pd/PPy-SDBS/Ti electrode during for 25min.
The Pd/PPy-SDBS/Ti electrode washing is clean, place 0.5mol/L H 2SO 4In the solution, be counter electrode with the platinized platinum, with Hg/Hg 2SO 4Electrode is that reference electrode carries out cyclic voltammetry scan.The electric potential scanning scope is-700mV～700mV that sweep velocity is 50mV/s.The gained cyclic voltammetry curve is seen the c among Fig. 1, the hydrogen adsorption peak occurs about-600mV, and peak point current is-99.33mA.
Embodiment 4
1) takes by weighing PdCl 2Powder is dissolved in the 3mol/L HCl solution, adds the PdCl that deionized water is mixed with 25mmol/L 2Solution;
2) titanium is embathed 3min remove surperficial thing in 0.5mol/L sulfuric acid after, successively in acetone (oil removing) and redistilled water respectively ultrasonic oscillation 15min to clean up dry for standby;
3) with the pyrroles with after the sulfuric acid of 0.3mol/L mixed in 7: 1000 by volume, add Sodium dodecylbenzene sulfonate and obtain mixing solutions, the content of Sodium dodecylbenzene sulfonate is 0.002g/mL in the mixing solutions;
4) with step 2) in titanium after handling be anode, platinized platinum is a negative electrode, is electrolytic solution with the solution of preparing in the step 3), adopts the method for galvanic deposit to make the PPy-SDBS/Ti electrode, depositing current density is 0.625mA/cm 2, depositing time is 5min;
5) be negative electrode with the PPy-SDBS/Ti electrode, platinized platinum is an anode, with the PdCl for preparing in the step 1) 2Solution is electrolytic solution, and adopting the method for galvanic deposit is 2.500mA/cm in depositing current density 2, depositing time makes the Pd/PPy-SDBS/Ti electrode during for 35min.
The Pd/PPy-SDBS/Ti electrode washing is clean, place 0.5mol/L H 2SO 4In the solution, be counter electrode with the platinized platinum, with Hg/Hg 2SO 4Electrode is that reference electrode carries out cyclic voltammetry scan.The electric potential scanning scope is-700mV～700mV that sweep velocity is 50mV/s.The gained cyclic voltammetry curve is seen a among Fig. 2, the hydrogen adsorption peak occurs about-600mV, and peak point current is-95.80mA.
Embodiment 5
1) takes by weighing PdCl 2Powder is dissolved in the 3mol/L HCl solution, adds the PdCl that deionized water is mixed with 20mmol/L 2Solution;
2) titanium is embathed 1min remove surperficial thing in 0.5mol/L sulfuric acid after, successively in acetone (oil removing) and redistilled water respectively ultrasonic oscillation 10min to clean up dry for standby;
3) with the pyrroles with after the sulfuric acid of 0.3mol/L mixed in 7: 1000 by volume, add Sodium dodecylbenzene sulfonate and obtain mixing solutions, the content of Sodium dodecylbenzene sulfonate is 0.0005g/mL in the mixing solutions;
4) with step 2) in titanium after handling be anode, platinized platinum is a negative electrode, is electrolytic solution with the solution of preparing in the step 3), adopts the method for galvanic deposit to make the PPy-SDBS/Ti electrode, depositing current density is 0.625mA/cm 2, depositing time is 5min;
5) be negative electrode with the PPy-SDBS/Ti electrode, platinized platinum is an anode, with the PdCl for preparing in the step 1) 2Solution is electrolytic solution, and adopting the method for galvanic deposit is 5.000mA/cm in depositing current density 2, depositing time makes the Pd/PPy-SDBS/Ti electrode during for 30min.
The Pd/PPy-SDBS/Ti electrode washing is clean, place 0.5mol/L H 2SO 4In the solution, be counter electrode with the platinized platinum, with Hg/Hg 2SO 4Electrode is that reference electrode carries out cyclic voltammetry scan.The electric potential scanning scope is-700mV～700mV that sweep velocity is 50mV/s.The gained cyclic voltammetry curve is seen the b among Fig. 2, the hydrogen adsorption peak occurs about-600mV, and peak point current is-105.12mA.
Comparative Examples
1) takes by weighing PdCl 2Powder is dissolved in the 3mol/L HCl solution, adds the PdCl that deionized water is mixed with 20mmol/L 2Solution;
2) titanium is embathed 1min remove surperficial thing in 0.5mol/L sulfuric acid after, successively in acetone (oil removing) and redistilled water respectively ultrasonic oscillation 10min to clean up dry for standby;
3) pyrroles was mixed with the sulfuric acid of 0.3mol/L in 7: 1000 by volume;
4) with step 2) in titanium after handling be anode, platinized platinum is a negative electrode, is electrolytic solution with the solution of preparing in the step 3), adopts the method for galvanic deposit to make the PPy/Ti electrode, depositing current density is 0.625mA/cm 2, depositing time is 5min;
5) be negative electrode with the PPy/Ti electrode, platinized platinum is an anode, with the PdCl for preparing in the step 1) 2Solution is electrolytic solution, and adopting the method for galvanic deposit is 5.000mA/cm in depositing current density 2, depositing time makes the Pd/PPy/Ti electrode during for 30min.
The Pd/PPy/Ti electrode washing is clean, place 0.5moL/LH 2SO 4In the solution, be counter electrode with the platinized platinum, with Hg/Hg 2SO 4Electrode is that reference electrode carries out cyclic voltammetry scan.The electric potential scanning scope is 700mV～700mV, and sweep velocity is 50mV/s.C among gained cyclic voltammetry curve such as Fig. 2, the hydrogen adsorption peak that about-600mV, occurs, peak point current is-52.14mA.
The result of embodiment and Comparative Examples comparison shows that the introducing of tensio-active agent has strengthened the catalytic activity of electrode, the cyclic voltammetric test shows, and the Pd/PPy-SDBS/Ti electrode has bigger hydrogen adsorption peak point current, has better dechlorination potential.

Claims (2)

1. the preparation method of a sodium dodecyl benzene sulfonate-doped titanium catalysis electrode is characterized in that, may further comprise the steps:
1) with Palladous chloride PdCl 2Powder is dissolved in the 3mol/L hydrochloric acid, with deionized water dilute the PdCl of 20～25mmol/L 2Solution;
2) titanium is soaked 1～3min in 0.5mol/L sulfuric acid after, ultrasonic oscillation 10～15min respectively in acetone and redistilled water successively, dry for standby;
3) pyrroles Py was mixed with the sulfuric acid of 0.3mol/L in 7: 1000 by volume, add Sodium dodecylbenzene sulfonate SDBS again and obtain mixing solutions, the content of Sodium dodecylbenzene sulfonate is 0.0005～0.002g/mL in the mixing solutions;
4) with step 2) in the oven dry after titanium be anode, platinized platinum is a negative electrode, is electrolytic solution with the mixing solutions of preparing in the step 3), galvanic deposit makes polypyrrole (Sodium dodecylbenzene sulfonate)/titanium electrode (PPy-SDBS/Ti electrode), depositing current density is 0.625mA/cm 2, depositing time is 5min;
5) the PPy-SDBS/Ti electrode that makes with step 4) is a negative electrode, and platinized platinum is an anode, with the PdCl of step 1) preparation 2Solution is electrolytic solution, and galvanic deposit makes sodium dodecyl benzene sulfonate-doped titanium Pd/PPy-SDBS/Ti catalysis electrode, and depositing current density is 2.500～5.000mA/cm 2, depositing time is 25～35min.
2. preparation method according to claim 1 is characterized in that, the depositing current density described in the step 5) is 2.500mA/cm 2, depositing time is 30min.
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CN106947990A (en) * 2017-03-13 2017-07-14 北京工业大学 A kind of electrophoresis pulse deposition prepares the method that graphene modified carries palladium electrode
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