CN1544930A - Method for detecting electrochemistry hydrogenation and electric energy symbiosis property of unsaturated organic acid and alcohol - Google Patents
Method for detecting electrochemistry hydrogenation and electric energy symbiosis property of unsaturated organic acid and alcohol Download PDFInfo
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- CN1544930A CN1544930A CNA2003101088952A CN200310108895A CN1544930A CN 1544930 A CN1544930 A CN 1544930A CN A2003101088952 A CNA2003101088952 A CN A2003101088952A CN 200310108895 A CN200310108895 A CN 200310108895A CN 1544930 A CN1544930 A CN 1544930A
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Abstract
The invention is a testing method of characteristics of electrochemical hydrogenation and electric energy symbiosis of unsaturated organic acid and alcohol, utilizing electrochemical circulating volt-ampere method of the typical three-electrode system, testing the characteristics of electrochemical hydrogenation and electric energy symbiosis of water-soluble unsaturated organic acid and alcohol in proton exchange film fuel battery reactor. It uses sulphuric acid solution of organic acid and alcohol at 0.01mol/L as electrolyte, smooth Pt electrode as research electrode, Pt wire as contrast electrode and reversible hydrogen electrode as reference electrode, in the range of scanning potential of 0-1.5V, determining the circulating volt-ampere curve of the sulphuric acid solution, examining the electrochemical reduction characteristics of different water-soluble organic acids and alcohols according to the potential value of reduction current. It has simple operation, low cost, short consumed time and highly repeated experimental results, and has an important significance in electrochemical hydrogenation of proton exchange film fuel batteries.
Description
Technical field:
The present invention relates to a kind of unsaturated organic acid and pure electrochemical hydrogenation and electric energy symbiotic characteristic method of testing, with electrochemical cyclic voltammetry, test is water-soluble unsaturated organic acid and pure electrochemical reduction characteristic of carrying out electrochemical hydrogenation and electric energy symbiosis in the Proton Exchange Membrane Fuel Cells reactor.Belong to the Electrochemical Engineering technical field.
Background technology:
Fuel cell is a kind ofly by the electrode catalyst course of reaction chemical energy to be converted into the electrochemical reaction appts of electric energy, and wherein Proton Exchange Membrane Fuel Cells (PEMFC) has shown the applications well prospect on electric automobile, small-sized portable power source.At present, people are promoting the business-like while of PEMFC, are also considering the application of PEMFC in wide spectrum more, and utilizing Proton Exchange Membrane Fuel Cells is one of its application direction as synthesis reactor.Utilize the fuel cell reaction device not only can generate chemicals, produce electric energy simultaneously, can also control reaction process easily by the load of control external circuit, pollute for a short time, meet the direction of environmental friendliness chemical technology research, the more important thing is, it can generate electricity, the resource utilization height.
Utilize Proton Exchange Membrane Fuel Cells, Kiyoshi Otsuka etc. has studied synthetic (the Kiyoshi Otsuka of a step of hydrogen peroxide, Ichiro Yamanaka.One step synthesis of hydrogen peroxidethrough fuel cell reaction, Electrochimica Acta, 1990,35 (2): 319-322), in the process of synthesize hydrogen peroxide, obtained 4-12mA/cm
2Current density.In same device, people such as Kiyoshi Otsuka have also studied the oxidation step of benzene.People such as Yuan Xiaozi also utilize Proton Exchange Membrane Fuel Cells to study nitrobenzene (Yuan Xiao-Zi, Ma Zi-Feng, Jiang Qi-Zhong et al, Cogeneration ofcyclohexylamine and electrical power using PEM fuel cell reactor, ElectrochemistryCommunications, 2001,3 (11): 599-602) and vinylcarbinol (Yuan Xiao-Zi, He Qing-Gang, Ma Zi-Feng et al, Electro-generative hydrogenation of allyl alcohol applying PEMfuel cell reactor, Electrochemistry Communications, 2003,5 (2): 189-193) and electrochemical hydrogenation and the electric energy symbiosis of unsaturated organic acid and alcohol react, in the hydrogeneration processes product, obtained certain electric current.
At present, the hydrogenation reaction activity of estimating material in the Proton Exchange Membrane Fuel Cells mainly is by cell reaction, measures open-circuit voltage and battery operated curve, i.e. current density-voltage curve that material reacts in fuel cell.The result who measures depends on multiple factor, as the brushing of electrode, the pressing of membrane electrode, the assembling of fuel cell, the sealing of battery and the control of reaction conditions etc.On the one hand, because the anode and cathode catalyzer in the membrane electrode all adopts noble metal, is generally the Pt/C catalyzer, PEM adopts the Nafion perfluoro sulfonic acid membrane, the cost of measuring hydrogenation activity by the operation of fuel cells curve is higher, and electrode production process is complicated.On the other hand, because measurement result is subjected to multiple controlling factors, battery operated curve repeated bad makes that result's reliability is also unsatisfactory.
Summary of the invention:
The object of the present invention is to provide a kind of unsaturated organic acid and pure electrochemical hydrogenation and electric energy symbiotic characteristic method of testing, solve existing method of testing cost height, length consuming time, the problem of experimental result unreliability provides effective research method for Proton Exchange Membrane Fuel Cells in the broader applications aspect the electrochemical hydrogenation simultaneously.
For reaching such purpose, the present invention utilizes typical galvanochemistry three-electrode system to measure different water-soluble unsaturated organic acids and the galvanochemistry cyclic voltammetry curve of alcohol in 1mol/L sulfuric acid.In cyclic voltammetric is measured, with the smooth platinum electrode is the research electrode, platinum filament is to electrode, reversible hydrogen electrode is a contrast electrode, with the organic acid of 0.01mol/L and the sulfuric acid solution of alcohol is electrolytic solution, sets given voltage by potentiostat, in 0V～1.5V scanning potential range, measure the organic acid of 0.01mol/L and the cyclic voltammetry curve of the sulfuric acid solution of alcohol, investigate the electrochemical reduction characteristic of different water-soluble organic acids and alcohol according to the potential value that reduction current occurs.
Concrete steps of the present invention are as follows:
(1) electrolytic cell carefully being cleaned back (ultrapure distilled water) in boiling water boiled 1 hour at least.
(2) with 1mol/L H
2SO
4Solution is electrolyte, and water-soluble organic acid and the alcoholic solution of configuration 0.01mol/L, solution are all with ultrapure distilled water configuration (＞17M Ω).
(3) with the smooth platinum electrode be the research electrode, platinum filament is to electrode, and reversible hydrogen electrode is a contrast electrode, will study electrode, be that 1: 1 the hydrogen peroxide and the mixed solution of the concentrated sulphuric acid are handled to electrode and contrast electrode volume ratio, removing surface impurity, and reversible hydrogen electrode is activated.
(4) solution and electrode are put into electrolytic cell, and electrode and potentiostat are connected.
(5) for eliminating the influence of oxygen to kinetic current, with nitrogen the solution in the electrolytic cell was purged before test, the time is about half an hour.
(6) test is carried out under room temperature and blanket of nitrogen.Setting the cyclic voltammetry scan voltage range is 0V～1.5V, and sweep velocity is 50mV/s.Measure cyclic voltammetry curve, get the 5th circulation result.
The present invention is simple to operate, and cost is low, weak point consuming time, and the repeatability of experimental result is high.Hydrogenation and the evaluation of electric energy symbiosis response characteristic that is embodied as in Proton Exchange Membrane Fuel Cells of the present invention provides a simple and effective method, and be significant in the broader applications aspect the electrochemical hydrogenation to Proton Exchange Membrane Fuel Cells.
Description of drawings:
Fig. 1 is 0.01mol/L vinylcarbinol 1mol/L H on the Pt electrode of the embodiment of the invention 1
2SO
4In cyclic voltammogram.
Fig. 2 is 0.01mol/L acrylic acid 1mol/L H on the Pt electrode of the embodiment of the invention 2
2SO
4In cyclic voltammogram.
Fig. 3 is 0.01mol/L crotonic acid 1mol/L H on the Pt electrode of the embodiment of the invention 3
2SO
4In cyclic voltammogram.
Embodiment:
Below by specific embodiment technical scheme of the present invention is further described.
Embodiment 1:
Configuration 1mol/L H
2SO
4Solution, and use 1mol/L H
2SO
4The vinylcarbinol solution of configuration 0.01mol/L, solution are all with ultrapure distilled water configuration (＞17M Ω).To study electrode ( 4mm, 99.95%, EG﹠amp; G), electrode (99.95%) and contrast electrode (reversible hydrogen electrode RHE) are handled with the mixed solution (volume ratio 1: 1) of the hydrogen peroxide and the concentrated sulphuric acid, removing surface impurity, and reversible hydrogen electrode is activated.Solution and electrode are put into electrolytic cell, and with electrode and potentiostat (EG﹠amp; G, Model 263 A) connect the back and feed nitrogen.The cyclic voltammetry scan program is set, and setting given voltage scan range is 0V～1.5V, and sweep velocity is 50mV/s.Measure cyclic voltammetry curve, get the 5th circulation result, the result as shown in Figure 1, the reduction current that begins to occur about the about 100mV of current potential is the reduction of vinylcarbinol, this positive potential is the driving force of hydrogenation reaction in the fuel cell.
Embodiment 2:
Configuration 1mol/L H
2SO
4Solution, and use 1mol/L H
2SO
4The acrylic acid solution of configuration 0.01mol/L, solution are all with ultrapure distilled water configuration (＞17M Ω).To study electrode ( 4mm, 99.95%, EG﹠amp; G), electrode (99.95%) and contrast electrode (reversible hydrogen electrode RHE) are handled with the mixed solution (volume ratio 1: 1) of the hydrogen peroxide and the concentrated sulphuric acid, removing surface impurity, and reversible hydrogen electrode is activated.Solution and electrode are put into electrolytic cell, and with electrode and potentiostat (EG﹠amp; G, Model 263 A) connect the back and feed nitrogen.The cyclic voltammetry scan program is set, and setting given voltage scan range is 0V～1.5V, and sweep velocity is 50mV/s.Measure cyclic voltammetry curve, get the 5th circulation result, the result as shown in Figure 2, the reduction current that begins to occur about the about 80mV of current potential is acrylic acid reduction, this positive potential is the driving force of hydrogenation reaction in the fuel cell.
Embodiment 3:
Configuration 1mol/L H
2SO
4Solution, and use 1mol/L H
2SO
4The crotonic acid solution of configuration 0.01mol/L, solution are all with ultrapure distilled water configuration (＞17M Ω).To study electrode ( 4mm, 99.95%, EG﹠amp; G), electrode (99.95%) and contrast electrode (reversible hydrogen electrode RHE) are handled with the mixed solution (volume ratio 1: 1) of the hydrogen peroxide and the concentrated sulphuric acid, removing surface impurity, and reversible hydrogen electrode is activated.Solution and electrode are put into electrolytic cell, and with electrode and potentiostat (EG﹠amp; G, Model 263 A) connect the back and feed nitrogen.The cyclic voltammetry scan program is set, and setting given voltage scan range is 0V～1.5V, and sweep velocity is 50mV/s.Measure cyclic voltammetry curve, get the 5th circulation result, the result as shown in Figure 3, the reduction current that begins to occur about the about 50mV of current potential is the reduction of crotonic acid, this positive potential is the driving force of hydrogenation reaction in the fuel cell.
Claims (1)
1, a kind of unsaturated organic acid and pure electrochemical hydrogenation and electric energy symbiotic characteristic method of testing is characterized in that comprising following concrete steps:
1) with 1mol/L H
2SO
4Solution is electrolyte, with ultrapure distilled water configuration concentration be 0.01mol/L water-soluble organic acid and alcoholic solution;
2) be the research electrode with the smooth platinum electrode, platinum filament is to electrode, and reversible hydrogen electrode is a contrast electrode, is that 1: 1 the hydrogen peroxide and the mixed solution of the concentrated sulphuric acid are handled with three electrode volume ratios, removes surface impurity and reversible hydrogen electrode is activated;
3) solution and electrode are put into electrolytic cell, and electrode and potentiostat are connected;
4) test is carried out under room temperature and blanket of nitrogen, and setting the cyclic voltammetry scan voltage range is 0V～1.5V, and sweep velocity is 50mV/s, measures cyclic voltammetry curve, gets the 5th circulation result.
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| Application Number | Priority Date | Filing Date | Title |
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| CNA2003101088952A CN1544930A (en) | 2003-11-27 | 2003-11-27 | Method for detecting electrochemistry hydrogenation and electric energy symbiosis property of unsaturated organic acid and alcohol |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1912610B (en) * | 2005-08-12 | 2011-11-16 | 深圳富泰宏精密工业有限公司 | Investigating method of metal ion concentration |
-
2003
- 2003-11-27 CN CNA2003101088952A patent/CN1544930A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1912610B (en) * | 2005-08-12 | 2011-11-16 | 深圳富泰宏精密工业有限公司 | Investigating method of metal ion concentration |
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