CN1544930A - Test method for electrochemical hydrogenation and electrical energy symbiosis of unsaturated organic acids and alcohols - Google Patents
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- 238000005984 hydrogenation reaction Methods 0.000 title claims abstract description 20
- 150000007524 organic acids Chemical class 0.000 title claims abstract description 17
- 238000010998 test method Methods 0.000 title claims abstract description 5
- 150000001298 alcohols Chemical class 0.000 title abstract description 11
- 235000005985 organic acids Nutrition 0.000 title abstract description 10
- 230000031068 symbiosis, encompassing mutualism through parasitism Effects 0.000 title abstract description 6
- 238000002484 cyclic voltammetry Methods 0.000 claims abstract description 19
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 17
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 14
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000001257 hydrogen Substances 0.000 claims abstract description 12
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 12
- 230000002441 reversible effect Effects 0.000 claims abstract description 12
- 238000011160 research Methods 0.000 claims abstract description 9
- 238000012360 testing method Methods 0.000 claims abstract description 6
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 5
- 239000003792 electrolyte Substances 0.000 claims abstract description 4
- 239000000243 solution Substances 0.000 claims description 23
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 239000012153 distilled water Substances 0.000 claims description 6
- 239000012535 impurity Substances 0.000 claims description 5
- 239000011259 mixed solution Substances 0.000 claims description 5
- 230000001476 alcoholic effect Effects 0.000 claims 1
- 229910052757 nitrogen Inorganic materials 0.000 claims 1
- 235000011149 sulphuric acid Nutrition 0.000 claims 1
- 239000001117 sulphuric acid Substances 0.000 claims 1
- 239000000446 fuel Substances 0.000 abstract description 20
- 239000012528 membrane Substances 0.000 abstract description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 abstract description 6
- XXROGKLTLUQVRX-UHFFFAOYSA-N allyl alcohol Chemical compound OCC=C XXROGKLTLUQVRX-UHFFFAOYSA-N 0.000 description 8
- 238000006243 chemical reaction Methods 0.000 description 7
- 238000000034 method Methods 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 4
- 229910001873 dinitrogen Inorganic materials 0.000 description 4
- 238000003786 synthesis reaction Methods 0.000 description 4
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 3
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- LDHQCZJRKDOVOX-NSCUHMNNSA-N crotonic acid Chemical compound C\C=C\C(O)=O LDHQCZJRKDOVOX-NSCUHMNNSA-N 0.000 description 3
- LDHQCZJRKDOVOX-UHFFFAOYSA-N trans-crotonic acid Natural products CC=CC(O)=O LDHQCZJRKDOVOX-UHFFFAOYSA-N 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 2
- PAFZNILMFXTMIY-UHFFFAOYSA-N cyclohexylamine Chemical compound NC1CCCCC1 PAFZNILMFXTMIY-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 230000005518 electrochemistry Effects 0.000 description 2
- LQNUZADURLCDLV-UHFFFAOYSA-N nitrobenzene Chemical compound [O-][N+](=O)C1=CC=CC=C1 LQNUZADURLCDLV-UHFFFAOYSA-N 0.000 description 2
- 229920000557 Nafion® Polymers 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 230000001680 brushing effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000001311 chemical methods and process Methods 0.000 description 1
- 238000003487 electrochemical reaction Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- UQSQSQZYBQSBJZ-UHFFFAOYSA-N fluorosulfonic acid Chemical compound OS(F)(=O)=O UQSQSQZYBQSBJZ-UHFFFAOYSA-N 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 230000036647 reaction Effects 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
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Abstract
一种不饱和有机酸和醇电化学加氢与电能共生特性测试方法，利用典型三电极系统的电化学循环伏安法，测试在质子交换膜燃料电池反应器中水溶性不饱和有机酸和醇电化学加氢与电能共生的特性。以0.01mol/L的有机酸和醇的硫酸溶液为电解液，以光滑铂电极为研究电极，铂丝为对电极，可逆氢电极为参比电极，在0V～1.5V扫描电位范围内，测定0.01mol/L的有机酸和醇的硫酸溶液的循环伏安曲线，根据出现还原电流的电位值来考察不同水溶性有机酸和醇的电化学还原特性。本发明操作简单，成本低，耗时短，实验结果的重复性高，对质子交换膜燃料电池在电化学加氢方面的更广泛应用有重要意义。
A test method for electrochemical hydrogenation and electric energy symbiosis of unsaturated organic acids and alcohols, using electrochemical cyclic voltammetry of a typical three-electrode system to test water-soluble unsaturated organic acids and alcohols in a proton exchange membrane fuel cell reactor The characteristics of the symbiosis of electrochemical hydrogenation and electrical energy. Using 0.01mol/L sulfuric acid solution of organic acid and alcohol as electrolyte, smooth platinum electrode as research electrode, platinum wire as counter electrode, and reversible hydrogen electrode as reference electrode, within the scanning potential range of 0V ~ 1.5V, measure The cyclic voltammetry curve of 0.01mol/L organic acid and alcohol sulfuric acid solution is used to investigate the electrochemical reduction characteristics of different water-soluble organic acids and alcohols according to the potential value of the reduction current. The invention has the advantages of simple operation, low cost, short time consumption and high repeatability of experimental results, and has great significance for wider application of proton exchange membrane fuel cells in electrochemical hydrogenation.
Description
技术领域：Technical field:
本发明涉及一种不饱和有机酸和醇电化学加氢与电能共生特性测试方法，以电化学循环伏安法，测试在质子交换膜燃料电池反应器中水溶性不饱和有机酸和醇进行电化学加氢与电能共生的电化学还原特性。属于电化学工程技术领域。The invention relates to a method for testing the electrochemical hydrogenation of unsaturated organic acids and alcohols and the symbiosis characteristics of electric energy. Electrochemical cyclic voltammetry is used to test the electric hydrogenation of water-soluble unsaturated organic acids and alcohols in a proton exchange membrane fuel cell reactor. Electrochemical reduction properties of symbiosis of chemical hydrogenation and electrical energy. It belongs to the technical field of electrochemical engineering.
背景技术：Background technique:
燃料电池是一种通过电极催化反应过程将化学能直接转化为电能的电化学反应装置，其中质子交换膜燃料电池(PEMFC)在电动汽车、小型移动电源上已展现出良好应用前景。目前，人们在促进PEMFC商业化的同时，也在考虑PEMFC在更广泛领域中的应用，利用质子交换膜燃料电池作为合成反应器是其应用方向之一。利用燃料电池反应器不仅能够生成化学品，同时产生电能，还可以通过控制外电路负载方便地控制反应进程，污染小，符合环境友好化学工艺研究的方向，更重要的是，它能够发电，资源利用率高。A fuel cell is an electrochemical reaction device that directly converts chemical energy into electrical energy through an electrode catalytic reaction process. Among them, the proton exchange membrane fuel cell (PEMFC) has shown good application prospects in electric vehicles and small mobile power sources. At present, while promoting the commercialization of PEMFC, people are also considering the application of PEMFC in a wider range of fields. Using proton exchange membrane fuel cells as synthesis reactors is one of its application directions. The use of fuel cell reactors can not only generate chemicals, but also generate electricity at the same time, and the reaction process can be conveniently controlled by controlling the external circuit load. The pollution is small, which is in line with the research direction of environmentally friendly chemical processes. More importantly, it can generate electricity and save resources. High utilization rate.
利用质子交换膜燃料电池，Kiyoshi Otsuka等研究了过氧化氢的一步合成(Kiyoshi Otsuka，Ichiro Yamanaka.One step synthesis of hydrogen peroxidethrough fuel cell reaction，Electrochimica Acta，1990，35(2)：319-322)，在合成过氧化氢的过程中得到了4-12mA/cm2的电流密度。在同样的装置中，Kiyoshi Otsuka等人还研究了苯的一步氧化。袁晓姿等人也利用质子交换膜燃料电池研究了硝基苯(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)和丙烯醇(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)以及不饱和有机酸和醇的电化学加氢与电能共生反应，在合成加氢产物的同时，得到了一定的的电流。Utilize the proton exchange membrane fuel cell, Kiyoshi Otsuka etc. have studied the one-step synthesis of hydrogen peroxide (Kiyoshi Otsuka, Ichiro Yamanaka.One step synthesis of hydrogen peroxide through fuel cell reaction, Electrochimica Acta, 1990,35(2):319-322), Current densities of 4-12 mA/ cm2 were obtained during the synthesis of hydrogen peroxide. In the same setup, Kiyoshi Otsuka et al. also studied the one-step oxidation of benzene. Yuan Xiaozi and others have also studied nitrobenzene (Yuan Xiao-Zi, Ma Zi-Feng, Jiang Qi-Zhong et al, Cogeneration of cyclohexylamine and electrical power using PEM fuel cell reactor, Electrochemistry Communications, 2001, 3( 11): 599-602) and allyl alcohol (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 the symbiotic reaction of electrochemical hydrogenation of unsaturated organic acids and alcohols with electric energy, while synthesizing hydrogenation products, a certain current was obtained.
目前，评价质子交换膜燃料电池中物质的加氢反应活性主要是通过电池反应，测定物质在燃料电池中反应的开路电压和电池工作曲线，即电流密度-电压曲线。测定的结果依赖于多种因素，如电极的涂刷、膜电极的压合、燃料电池的组装、电池的密封以及反应条件的控制等。一方面，由于膜电极中的阴阳极催化剂均采用贵金属，通常为Pt/C催化剂，质子交换膜采用Nafion全氟磺酸膜，通过燃料电池工作曲线来测定加氢活性的成本较高，而且电极制备过程较复杂。另一方面，由于测定结果受多种因素控制，电池工作曲线的重复性不好，使得结果的可靠性并不令人满意。At present, the evaluation of the hydrogenation reaction activity of the substance in the proton exchange membrane fuel cell is mainly through the battery reaction, and the open circuit voltage and the battery working curve of the substance reacted in the fuel cell are measured, that is, the current density-voltage curve. The results of the determination depend on many factors, such as the brushing of electrodes, the pressing of membrane electrodes, the assembly of fuel cells, the sealing of cells, and the control of reaction conditions. On the one hand, since the cathode and anode catalysts in the membrane electrodes are all made of noble metals, usually Pt/C catalysts, and the proton exchange membrane uses Nafion perfluorosulfonic acid membrane, the cost of measuring the hydrogenation activity through the fuel cell working curve is relatively high, and the electrode The preparation process is more complicated. On the other hand, since the measurement results are controlled by many factors, the repeatability of the battery working curve is not good, which makes the reliability of the results unsatisfactory.
发明内容：Invention content:
本发明的目的在于提供一种不饱和有机酸和醇电化学加氢与电能共生特性测试方法，解决现有测试方法成本高，耗时长，实验结果不可靠性的问题，同时为质子交换膜燃料电池在电化学加氢方面的更广泛应用提供有效的研究方法。The purpose of the present invention is to provide a test method for the electrochemical hydrogenation of unsaturated organic acids and alcohols and electric energy symbiosis characteristics, which solves the problems of high cost, long time consumption and unreliable experimental results of the existing test methods, and at the same time provides proton exchange membrane fuel The wider application of batteries in electrochemical hydrogenation provides effective research methods.
为达到这样的目的，本发明利用典型的电化学三电极体系测定不同水溶性不饱和有机酸和醇在1mol/L硫酸中的电化学循环伏安曲线。在循环伏安测定中，以光滑铂电极为研究电极，铂丝为对电极，可逆氢电极为参比电极，以0.01mol/L的有机酸和醇的硫酸溶液为电解液，通过恒电位仪设定给定电压，在0V～1.5V扫描电位范围内，测定0.01mol/L的有机酸和醇的硫酸溶液的循环伏安曲线，根据出现还原电流的电位值来考察不同水溶性有机酸和醇的电化学还原特性。To achieve such purpose, the present invention utilizes a typical electrochemical three-electrode system to measure the electrochemical cyclic voltammetry curves of different water-soluble unsaturated organic acids and alcohols in 1mol/L sulfuric acid. In the cyclic voltammetry, the smooth platinum electrode is used as the research electrode, the platinum wire is used as the counter electrode, the reversible hydrogen electrode is used as the reference electrode, and the sulfuric acid solution of organic acid and alcohol of 0.01mol/L is used as the electrolyte. Set a given voltage, and measure the cyclic voltammetry curve of 0.01mol/L organic acid and alcohol sulfuric acid solution within the scanning potential range of 0V ~ 1.5V, and investigate different water-soluble organic acids and alcohols according to the potential value of the reduction current. Electrochemical reduction properties of alcohols.
本发明的具体步骤如下：Concrete steps of the present invention are as follows:
(1)将电解池仔细洗净后在沸水中(超纯蒸馏水)煮至少1小时。(1) Wash the electrolytic cell carefully and boil it in boiling water (ultra-pure distilled water) for at least 1 hour.
(2)以1mol/L H2SO4溶液为电解质，配置0.01mol/L的水溶性有机酸和醇溶液，溶液均用超纯蒸馏水配置(＞17MΩ)。(2) Using 1mol/L H 2 SO 4 solution as electrolyte, prepare 0.01mol/L water-soluble organic acid and alcohol solution, all solutions are prepared with ultra-pure distilled water (>17MΩ).
(3)以光滑铂电极为研究电极，铂丝为对电极，可逆氢电极为参比电极，将研究电极、对电极和参比电极用体积比为1∶1的过氧化氢和浓硫酸的混合溶液进行处理，以除去表面杂质，并将可逆氢电极活化。(3) The smooth platinum electrode is used as the research electrode, the platinum wire is used as the counter electrode, and the reversible hydrogen electrode is used as the reference electrode. The mixed solution is treated to remove surface impurities and activate the reversible hydrogen electrode.
(4)将溶液及电极放入电解池，并将电极与恒电位仪接好。(4) Put the solution and the electrode into the electrolytic cell, and connect the electrode to the potentiostat.
(5)为消除氧气对反应电流的影响，在测试之前用氮气对电解池中的溶液进行吹扫，时间约为半小时。(5) In order to eliminate the influence of oxygen on the reaction current, the solution in the electrolytic cell was purged with nitrogen gas for about half an hour before the test.
(6)测试在室温以及氮气氛下进行。设定循环伏安扫描电压范围为0V～1.5V，扫描速度为50mV/s。测定循环伏安曲线，取第五循环结果。(6) The test was carried out at room temperature and under a nitrogen atmosphere. Set the range of cyclic voltammetry scanning voltage to 0V-1.5V, and the scanning speed to 50mV/s. Measure the cyclic voltammetry curve, and take the result of the fifth cycle.
本发明操作简单，成本低，耗时短，实验结果的重复性高。本发明的实施为在质子交换膜燃料电池中的加氢与电能共生反应特性评价提供了一个简便而有效的方法，对质子交换膜燃料电池在电化学加氢方面的更广泛应用有重要意义。The invention has the advantages of simple operation, low cost, short time consumption and high repeatability of experimental results. The implementation of the invention provides a simple and effective method for evaluating the symbiotic reaction characteristics of hydrogenation and electric energy in the proton exchange membrane fuel cell, and is of great significance to the wider application of the proton exchange membrane fuel cell in electrochemical hydrogenation.
附图说明：Description of drawings:
图1为本发明实施例1的0.01mol/L丙烯醇在Pt电极上1mol/L H2SO4中的循环伏安图。Fig. 1 is a cyclic voltammogram of 0.01 mol/L allyl alcohol in 1 mol/L H 2 SO 4 on a Pt electrode in Example 1 of the present invention.
图2为本发明实施例2的0.01mol/L丙烯酸在Pt电极上1mol/L H2SO4中的循环伏安图。Fig. 2 is a cyclic voltammogram of 0.01 mol/L acrylic acid in 1 mol/L H 2 SO 4 on a Pt electrode in Example 2 of the present invention.
图3为本发明实施例3的0.01mol/L巴豆酸在Pt电极上1mol/L H2SO4中的循环伏安图。Fig. 3 is a cyclic voltammogram of 0.01 mol/L crotonic acid in 1 mol/L H 2 SO 4 on a Pt electrode in Example 3 of the present invention.
具体实施方式：Detailed ways:
以下通过具体的实施例对本发明的技术方案作进一步描述。The technical solution of the present invention will be further described below through specific examples.
实施例1：Example 1:
配置1mol/L H2SO4溶液，并用1mol/L H2SO4配置0.01mol/L的丙烯醇溶液，溶液均用超纯蒸馏水配置(＞17MΩ)。将研究电极(4mm，99.95％，EG&G)、对电极(99.95％)和参比电极(可逆氢电极RHE)用过氧化氢和浓硫酸的混合溶液(体积比1∶1)处理，以除去表面杂质，并将可逆氢电极活化。将溶液及电极放入电解池，并将电极与恒电位仪(EG&G，Model 263 A)接好后通入氮气。设置循环伏安扫描程序，设定给定电压扫描范围为0V～1.5V，扫描速度为50mV/s。测定循环伏安曲线，取第五循环结果，结果如图1所示，在电位约100mV左右开始出现的还原电流为丙烯醇的还原，此正电位即为燃料电池中加氢反应的驱动力。Prepare 1mol/L H 2 SO 4 solution, and use 1mol/L H 2 SO 4 to prepare 0.01mol/L acrylic alcohol solution. Both solutions are prepared with ultra-pure distilled water (>17MΩ). The research electrode (4 mm, 99.95%, EG&G), the counter electrode (99.95%) and the reference electrode (reversible hydrogen electrode RHE) were treated with a mixed solution of hydrogen peroxide and concentrated sulfuric acid (volume ratio 1:1) to remove surface impurities and activate the reversible hydrogen electrode. Put the solution and electrode into the electrolytic cell, connect the electrode to the potentiostat (EG&G, Model 263 A), and then pass nitrogen gas. Set the cyclic voltammetry scanning program, set the given voltage scanning range as 0V to 1.5V, and the scanning speed as 50mV/s. Measure the cyclic voltammetry curve, take the result of the fifth cycle, the result is shown in Figure 1, the reduction current that begins to appear at a potential of about 100mV is the reduction of allyl alcohol, and this positive potential is the driving force of the hydrogenation reaction in the fuel cell.
实施例2：Example 2:
配置1mol/L H2SO4溶液，并用1mol/L H2SO4配置0.01mol/L的丙烯酸溶液，溶液均用超纯蒸馏水配置(＞17MΩ)。将研究电极(4mm，99.95％，EG&G)、对电极(99.95％)和参比电极(可逆氢电极RHE)用过氧化氢和浓硫酸的混合溶液(体积比1∶1)处理，以除去表面杂质，并将可逆氢电极活化。将溶液及电极放入电解池，并将电极与恒电位仪(EG&G，Model 263 A)接好后通入氮气。设置循环伏安扫描程序，设定给定电压扫描范围为0V～1.5V，扫描速度为50mV/s。测定循环伏安曲线，取第五循环结果，结果如图2所示，在电位约80mV左右开始出现的还原电流为丙烯酸的还原，此正电位即为燃料电池中加氢反应的驱动力。Prepare 1mol/L H 2 SO 4 solution, and use 1mol/L H 2 SO 4 to prepare 0.01mol/L acrylic acid solution. Both solutions are prepared with ultra-pure distilled water (>17MΩ). The research electrode (4 mm, 99.95%, EG&G), the counter electrode (99.95%) and the reference electrode (reversible hydrogen electrode RHE) were treated with a mixed solution of hydrogen peroxide and concentrated sulfuric acid (volume ratio 1:1) to remove surface impurities and activate the reversible hydrogen electrode. Put the solution and electrode into the electrolytic cell, connect the electrode to the potentiostat (EG&G, Model 263 A), and then pass nitrogen gas. Set the cyclic voltammetry scanning program, set the given voltage scanning range as 0V to 1.5V, and the scanning speed as 50mV/s. Measure the cyclic voltammetry curve, take the result of the fifth cycle, the result is shown in Figure 2, the reduction current that begins to appear at a potential of about 80mV is the reduction of acrylic acid, and this positive potential is the driving force of the hydrogenation reaction in the fuel cell.
实施例3：Example 3:
配置1mol/L H2SO4溶液，并用1mol/L H2SO4配置0.01mol/L的巴豆酸溶液，溶液均用超纯蒸馏水配置(＞17MΩ)。将研究电极(4mm，99.95％，EG&G)、对电极(99.95％)和参比电极(可逆氢电极RHE)用过氧化氢和浓硫酸的混合溶液(体积比1∶1)处理，以除去表面杂质，并将可逆氢电极活化。将溶液及电极放入电解池，并将电极与恒电位仪(EG&G，Model 263 A)接好后通入氮气。设置循环伏安扫描程序，设定给定电压扫描范围为0V～1.5V，扫描速度为50mV/s。测定循环伏安曲线，取第五循环结果，结果如图3所示，在电位约50mV左右开始出现的还原电流为巴豆酸的还原，此正电位即为燃料电池中加氢反应的驱动力。Prepare 1mol/L H 2 SO 4 solution and 0.01 mol/L crotonic acid solution with 1 mol/L H 2 SO 4 , all solutions are prepared with ultra-pure distilled water (>17MΩ). The research electrode (4 mm, 99.95%, EG&G), the counter electrode (99.95%) and the reference electrode (reversible hydrogen electrode RHE) were treated with a mixed solution of hydrogen peroxide and concentrated sulfuric acid (volume ratio 1:1) to remove surface impurities and activate the reversible hydrogen electrode. Put the solution and electrode into the electrolytic cell, connect the electrode to the potentiostat (EG&G, Model 263 A), and then pass nitrogen gas. Set the cyclic voltammetry scanning program, set the given voltage scanning range as 0V to 1.5V, and the scanning speed as 50mV/s. Measure the cyclic voltammetry curve, take the result of the fifth cycle, the result is shown in Figure 3, the reduction current that begins to appear at a potential of about 50mV is the reduction of crotonic acid, and this positive potential is the driving force of the hydrogenation reaction in the fuel cell.
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