CN110988062B - Preparation method of gas diffusion electrode for measuring hydrogen sulfide gas - Google Patents
Preparation method of gas diffusion electrode for measuring hydrogen sulfide gas Download PDFInfo
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Abstract
The invention provides a preparation method of a gas diffusion electrode for measuring hydrogen sulfide gas, which comprises the steps of mixing a metal platinum salt precursor solution and a metal ruthenium salt precursor solution, then adding a surfactant and a reducing agent to react the metal platinum salt precursor solution and the metal ruthenium salt precursor solution, cooling, washing and centrifugally separating a product obtained by the reaction to obtain a catalyst precipitate; passivating the catalyst precipitate to obtain a passivated Pt-Ru alloy catalyst; mixing the passivated Pt-Ru alloy catalyst with a slow release agent and a hydrophobic fluorine-containing binder to prepare platinum-ruthenium alloy electrode slurry, mixing the platinum-ruthenium alloy electrode slurry with PTFE emulsion, and passivating and molding at the temperature of 280-300 ℃ to obtain the gas diffusion electrode. The preparation method can ensure that the alloy catalyst has higher catalytic activity and can prevent the catalyst from generating violent reaction in the using process, the response time is short, and the service life is long.
Description
Technical Field
The invention belongs to the technical field of gas detection, and particularly relates to a preparation method of a gas diffusion electrode for measuring hydrogen sulfide gas.
Background
Hydrogen sulfide gas is one of the main toxic and atmospheric pollutants in the fields of petroleum, natural gas, mining, chemical engineering and the like. The electrochemical hydrogen sulfide gas sensor is the most widely applied monitoring means at present. The electrochemical gas sensor mainly comprises a gas diffusion electrode, an electrolyte, a structural component and the like. At present, the electrochemical hydrogen sulfide sensor faces the main problems of long response time, short service life and the like. Of which the gas diffusion electrode is the main determining factor.
The diffusion electrode for the hydrogen sulfide electrochemical gas sensor mainly comprises a nano Pt-Ru alloy catalyst and a hydrophobic substance PTFE. The gas diffusion electrode is prepared by preparing an electronic slurry from a proper amount of a nano Pt-Ru alloy catalyst, a hydrophobic substance polytetrafluoroethylene, a dispersing agent such as terpineol and triton and the like, and performing printing, sintering, curing, press forming and other processes. The particle size of the selected nano Pt-Ru alloy catalyst is usually larger than 30nm, and a diffusion electrode prepared by the catalyst with larger particle size has larger resistance and electrode thickness, so that the response time of the sensor is prolonged; diffusion electrodes prepared with catalysts of larger particle size generally have poorer strength and are prone to breakage, resulting in shorter sensor life. Meanwhile, the catalyst with high activity still burns violently with oxygen in the electrode sintering process, thereby damaging the electrode micropores.
Disclosure of Invention
Accordingly, it is a need to provide a method for preparing a gas diffusion electrode for measuring hydrogen sulfide gas, so as to solve the above-mentioned problems.
The technical scheme provided by the invention is as follows: a preparation method of a gas diffusion electrode for measuring hydrogen sulfide gas specifically comprises the following steps:
reacting a metal platinum salt precursor solution and a metal ruthenium salt precursor solution according to a volume ratio of 1: (10-15), adding a surfactant and a reducing agent, reacting the metal platinum salt precursor solution with the metal ruthenium salt precursor solution under magnetic stirring, cooling, washing and centrifugally separating a product obtained by the reaction to obtain a catalyst precipitate; wherein the mass fraction of platinum-containing ions in the metal platinum salt precursor solution is 8-10%; the mass fraction of ruthenium ions in the metal ruthenium salt precursor solution is 5-13%;
passivating the catalyst precipitate for 12 to 48 hours in an environment with the temperature of between 110 and 130 ℃ and the oxygen concentration of between 3.0 and 5 percent to obtain a passivated Pt-Ru alloy catalyst; wherein the molar ratio of the Pt element to the Ru element in the passivated Pt-Ru alloy catalyst is 1: (5-15), wherein the grain size of the passivated Pt-Ru alloy catalyst is less than 10 nm;
forming, namely mixing the passivated Pt-Ru alloy catalyst with a slow release agent and a hydrophobic fluorine-containing binder to prepare platinum-ruthenium alloy electrode slurry, mixing the platinum-ruthenium alloy electrode slurry with PTFE emulsion, and carrying out passivation forming treatment at the temperature of 280-300 ℃ to obtain a gas diffusion electrode;
wherein the mass ratio of the passivated Pt-Ru alloy catalyst to the slow release agent to the hydrophobic fluorine-containing binder is 3: 1: (0.3-0.5).
The mol ratio of Pt element to Ru element in the passivated Pt-Ru alloy catalyst is 1: (5-15) mainly because: when the molar ratio of the Pt element to the Ru element is less than 1: 5, the electronic benefit generated between Ru and Pt cannot meet the binding force for overcoming agglomeration between particles, and when the molar ratio of Pt element to Ru element is more than 1: 15, impurities exist because the metal ruthenium salt precursor has too much Ru element to be completely reacted.
When the mass ratio of the passivated Pt-Ru alloy catalyst to the slow release agent to the hydrophobic fluorine-containing binder exceeds 3: 1: (0.3-0.5), the problems of excessive slow-release agent or insufficient slow-release agent and weak binding power between the slow-release agent and catalyst particles or complete coating of the slow-release agent and the catalyst particles by a binder exist, so that the balance between slow release and catalyst activity cannot be well balanced. When the slow release agent is excessive, the excessive slow release agent completely prevents oxygen from contacting with the naked catalyst, so that the activity of the catalyst is sharply reduced; when the slow release agent is insufficient, the naked catalyst can react with oxygen violently, so that micropores of the electrode are damaged. Therefore, the mass ratio of the passivated Pt-Ru alloy catalyst, the slow release agent and the hydrophobic fluorine-containing binder is limited to 3: 1: (0.3-0.5).
Based on the above, the metal ruthenium salt precursor solution is a ruthenium trichloride solution.
Based on the above, the metal platinum salt precursor solution is a chloroplatinic acid solution or a potassium chloroplatinate solution.
Based on the above, the surfactant is a polyvinylpyrrolidone water solution with the mass concentration of 0.02 g/ml; the reducing agent is a potassium borohydride aqueous solution with the mass concentration of 0.067 g/ml.
Based on the above, the slow release agent is one or a mixture of more of terpineol, polyethylene glycol, polyvinyl alcohol and carboxymethyl cellulose, and the hydrophobic fluorine-containing binder is one or a mixture of more of polychlorotrifluoroethylene emulsion, polytetrafluoroethylene emulsion, polyhexafluoropropylene emulsion or polyvinylidene fluoride emulsion.
Based on the above, the mass fraction of platinum-containing ions in the metal platinum salt precursor solution is 10%; the mass fraction of ruthenium ions in the metal ruthenium salt precursor solution is 10%.
Based on the above, the volume ratio of the metal platinum salt precursor solution to the metal ruthenium salt precursor solution is 1: 15.
wherein, the molar ratio of Pt element to Ru element in the passivated Pt-Ru alloy catalyst is 1: (5-15), so that the content of ruthenium ions in the reaction system is higher than that of platinum ions, d electrons of Pt enter a d orbit of Ru, and relatively more s electrons of Ru are fed back to the s orbit of Pt, and the final result is that the electron density of Pt is increased, the effective active site of Pt is increased, sufficient electronic benefit is generated between Ru and Pt, and the agglomeration phenomenon between nano particles is prevented. Meanwhile, the temperature and concentration unevenness in the liquid phase can be avoided under the magnetic stirring, and simultaneously, as the functional groups on the surface of the reducing agent are adsorbed to the functional groups through the platinum ions and the ruthenium ions in the coordination reaction or the ion exchange solution, the platinum ions and the ruthenium ions which interact with the functional groups become precursors, anchor points are provided for the subsequently generated fine alloy nanoparticles, and the agglomeration phenomenon among the nanoparticles is further prevented. Therefore, the grain diameter of the passivated Pt-Ru alloy catalyst prepared by the method can be less than 10 nm.
Compared with the prior art, the preparation method of the gas diffusion electrode for measuring the hydrogen sulfide gas, provided by the invention, has the advantages that the Pt-Ru alloy catalyst with the particle size smaller than 10nm is prepared, the Pt-Ru alloy catalyst is passivated, and a non-compact passivation layer is formed on the surface of the Pt-Ru alloy catalyst, so that the violent reaction of the catalyst in the use process is effectively avoided, the resistance of the electrode is obviously reduced, the thickness of the electrode is reduced, and the response time of the sensor is shortened. Furthermore, because the non-compact passivation layer is mainly a porous oxide layer, a slow release agent with a slow release effect is added during the preparation of the electrode, and the mass ratio of the passivated Pt-Ru alloy catalyst to the slow release agent to the hydrophobic fluorine-containing binder is defined as 3: 1: (0.3-0.5), the Pt-Ru alloy catalyst has high catalytic activity, oxygen can slowly contact with the exposed catalyst, severe reaction of the catalyst in the using process is further prevented, and damage to electrode micropores caused by severe oxidation of the electrode in the sintering process can be avoided.
Detection shows that compared with a gas diffusion electrode prepared by using a Pt-Ru alloy catalyst which is not passivated in the whole process and added with a slow release agent, the sintered electrode prepared by the invention has the following pore diameter range: 50 nm to 90 nm; the service life of the electrode is 200mA/cm 2 The current density of the current is increased from 2000hr to 3000hr to 4000hr, and the 30-second response amplitude is increased from 80% to 95%.
Drawings
FIG. 1 is a scanning electron microscope image of a passivated Pt-Ru alloy catalyst prepared by the preparation method provided by the invention.
Detailed Description
The technical solution of the present invention is further described in detail by the following embodiments.
Example 1
The embodiment of the invention provides a preparation method of a gas diffusion electrode for measuring hydrogen sulfide gas, which comprises the following steps:
mixing a metal platinum salt precursor solution and a metal ruthenium salt precursor solution, adding a surfactant and a reducing agent, reacting the metal platinum salt precursor solution and the metal ruthenium salt precursor solution, cooling, washing and centrifugally separating a product obtained by the reaction to obtain a catalyst precipitate;
passivating the catalyst precipitate to obtain a passivated Pt-Ru alloy catalyst;
and (2) forming, namely mixing the passivated Pt-Ru alloy catalyst with a slow release agent and a hydrophobic fluorine-containing binder to prepare platinum-ruthenium alloy electrode slurry, mixing the platinum-ruthenium alloy electrode slurry with PTFE emulsion, and carrying out passivation forming treatment at the temperature of 280 ℃ to obtain the gas diffusion electrode.
Wherein the passivation step comprises treating the catalyst precipitate for 24 hours at 130 ℃ in an environment with an oxygen concentration of 5%.
The metal ruthenium salt precursor solution is a ruthenium trichloride solution. The metal platinum salt precursor solution is a chloroplatinic acid solution. The surfactant is polyvinylpyrrolidone aqueous solution, and the reducing agent is potassium borohydride aqueous solution; the slow release agent is terpineol, and the hydrophobic fluorine-containing binder is polytetrafluoroethylene dispersion.
The mass fraction of platinum-containing ions in the metal platinum salt precursor solution is 8%; the mass fraction of ruthenium ions in the metal ruthenium salt precursor solution is 5%.
The volume ratio of the metal platinum salt precursor solution to the metal ruthenium salt precursor solution is 1: 10.
the mass ratio of the passivated Pt-Ru alloy catalyst to the slow release agent to the hydrophobic fluorine-containing binder is 3: 1: 0.3.
upon testing, as shown in FIG. 1, it can be seen that the particle size of the prepared passivated Pt-Ru alloy catalyst is less than 10nm, and the pore size range after sintering of the electrode prepared in this example is: 50 nm; the electrode life is 200mA/cm 2 At a current density of 4000hr, the 30 second response amplitude was 95%.
Example 2
The embodiment of the invention provides a preparation method of a gas diffusion electrode for measuring hydrogen sulfide gas, which comprises the following steps:
(1) weighing 20g of potassium borohydride and dissolving the potassium borohydride in 300ml of deionized water;
(2) take 1ml of H 2 PtCl 6 (containing Pt10%) into a 250ml beaker;
(3) adding 15ml of RuCl into a beaker 3 Diluting to 75ml, stirring thoroughly to obtain H 2 PtCl 6 And RuCl 3 Fully mixing the solution;
(4) weighing 2g of PVP (polyvinylpyrrolidone), weighing 100ml of deionized water by using a measuring cylinder, placing the deionized water in a 250ml beaker, stirring by using a magnetic stirrer until the PVP is completely dissolved, and adding the PVP into the beaker in the step 3;
(5) adding the substances in the step 1 into the substances in the step 4, and magnetically stirring for 20 min; and after stirring, taking down the magnetic stirrer, standing for 10min, pouring out supernatant into a 2000ml beaker, washing the precipitate until no chloride ion is detected, and passivating the precipitate at 125 ℃ under the environment of oxygen concentration of 4.2% for 24 hours to obtain the Pt-Ru alloy catalyst.
(6) And mixing the passivated Pt-Ru alloy catalyst with a slow release agent and a hydrophobic fluorine-containing binder to prepare platinum-ruthenium alloy electrode slurry, mixing the platinum-ruthenium alloy electrode slurry with PTFE emulsion, and carrying out passivation molding treatment at the temperature of 280 ℃ to obtain the gas diffusion electrode.
Wherein the platinum-ruthenium alloy electrode slurry comprises the following components in proportion of Pt-Ru: sustained release agent: hydrophobic fluorine-containing binder = 3: 1: 0.5.
tests show that the particle size of the passivated Pt-Ru alloy catalyst prepared in the embodiment is less than 10nm, and the pore diameter range of the sintered electrode prepared in the embodiment is as follows: 60 nm; the service life of the electrode is 200mA/cm 2 The current density of (2) was 3500hr, and the 30-second response amplitude was 90%.
Example 3
The embodiment of the invention provides a preparation method of a gas diffusion electrode for measuring hydrogen sulfide gas, which comprises the following steps:
mixing a metal platinum salt precursor solution and a metal ruthenium salt precursor solution, adding a surfactant and a reducing agent, reacting the metal platinum salt precursor solution and the metal ruthenium salt precursor solution, cooling, washing and centrifugally separating a product obtained by the reaction to obtain a catalyst precipitate;
passivating the catalyst precipitate to obtain a passivated Pt-Ru alloy catalyst;
and (2) forming, namely mixing the passivated Pt-Ru alloy catalyst with a slow release agent and a hydrophobic fluorine-containing binder to prepare platinum-ruthenium alloy electrode slurry, mixing the platinum-ruthenium alloy electrode slurry with PTFE emulsion, and carrying out passivation forming treatment at 290 ℃ to obtain the gas diffusion electrode.
Wherein the passivating step comprises the step of treating the catalyst precipitate for 12 hours at 130 ℃ under the environment with the oxygen concentration of 3.0%. The metal ruthenium salt precursor solution is a ruthenium trichloride solution.
The metal platinum salt precursor solution is a potassium chloroplatinate solution. The surfactant is polyvinylpyrrolidone aqueous solution; the reducing agent is a potassium borohydride aqueous solution; the slow release agent is carboxymethyl cellulose, and the hydrophobic fluorine-containing binder is polychlorotrifluoroethylene emulsion.
The mass fraction of platinum-containing ions in the metal platinum salt precursor solution is 10%; the mass fraction of ruthenium ions in the metal ruthenium salt precursor solution is 5%.
The volume ratio of the metal platinum salt precursor solution to the metal ruthenium salt precursor solution is 1: 12. the mass ratio of the passivated Pt-Ru alloy catalyst to the slow release agent to the hydrophobic fluorine-containing binder is 3: 1: 0.4.
tests show that the particle size of the passivated Pt-Ru alloy catalyst prepared in the embodiment is less than 10nm, and the pore diameter range of the sintered electrode prepared in the embodiment is as follows: 70 nm; the electrode life is 200mA/cm 2 At a current density of 3000hr, the 30 second response amplitude was 80%.
Finally, it should be noted that: the above examples are only intended to illustrate the technical solution of the present invention and not to limit it; although the present invention has been described in detail with reference to preferred embodiments, those skilled in the art will understand that: modifications to the specific embodiments of the invention or equivalent substitutions for parts of the technical features may be made; without departing from the spirit of the invention, it is intended to cover all modifications within the scope of the invention as claimed.
Claims (6)
1. A preparation method of a gas diffusion electrode for measuring hydrogen sulfide gas specifically comprises the following steps:
reacting a metal platinum salt precursor solution and a metal ruthenium salt precursor solution according to a volume ratio of 1: (10-15), adding a surfactant and a reducing agent, reacting the metal platinum salt precursor solution with the metal ruthenium salt precursor solution under magnetic stirring, cooling, washing and centrifugally separating a product obtained by the reaction to obtain a catalyst precipitate; wherein the mass fraction of platinum-containing ions in the metal platinum salt precursor solution is 8-10%; the mass fraction of ruthenium ions in the metal ruthenium salt precursor solution is 5-13%;
passivating the catalyst precipitate for 12 to 48 hours in an environment with the temperature of between 110 and 130 ℃ and the oxygen concentration of between 3.0 and 5 percent to obtain a passivated Pt-Ru alloy catalyst; wherein the molar ratio of the Pt element to the Ru element in the passivated Pt-Ru alloy catalyst is 1: (5-15), wherein the grain size of the passivated Pt-Ru alloy catalyst is less than 10 nm;
forming, namely mixing the passivated Pt-Ru alloy catalyst with a slow release agent and a hydrophobic fluorine-containing binder to prepare platinum-ruthenium alloy electrode slurry, mixing the platinum-ruthenium alloy electrode slurry with PTFE emulsion, and carrying out passivation forming treatment at the temperature of 280-300 ℃ to obtain a gas diffusion electrode;
wherein the mass ratio of the passivated Pt-Ru alloy catalyst to the slow release agent to the hydrophobic fluorine-containing binder is 3: 1: (0.3-0.5); the slow release agent is one or a mixture of more of terpineol, polyethylene glycol, polyvinyl alcohol and carboxymethyl cellulose, and the hydrophobic fluorine-containing binder is one or a mixture of more of polychlorotrifluoroethylene emulsion, polytetrafluoroethylene emulsion, polyhexafluoropropylene emulsion or polyvinylidene fluoride emulsion.
2. The gas diffusion electrode production method for measuring hydrogen sulfide gas according to claim 1, characterized in that: the metal ruthenium salt precursor solution is a ruthenium trichloride solution.
3. The gas diffusion electrode production method for measuring hydrogen sulfide gas as claimed in claim 2, wherein: the metal platinum salt precursor solution is a chloroplatinic acid solution or a potassium chloroplatinate solution.
4. The gas diffusion electrode production method for measuring hydrogen sulfide gas according to claim 3, characterized in that: the surfactant is polyvinylpyrrolidone water solution with the mass concentration of 0.02 g/ml; the reducing agent is a potassium borohydride aqueous solution with the mass concentration of 0.067 g/ml.
5. The gas diffusion electrode production method for measuring hydrogen sulfide gas according to claim 4, characterized in that: the mass fraction of platinum-containing ions in the metal platinum salt precursor solution is 10%; the mass fraction of ruthenium ions in the metal ruthenium salt precursor solution is 10%.
6. The gas diffusion electrode production method for measuring hydrogen sulfide gas as claimed in claim 5, wherein: the volume ratio of the metal platinum salt precursor solution to the metal ruthenium salt precursor solution is 1: 15.
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| GB2167192A (en) * | 1984-11-15 | 1986-05-21 | Atomic Energy Authority Uk | Gas sensor |
| US5173166A (en) * | 1990-04-16 | 1992-12-22 | Minitech Co. | Electrochemical gas sensor cells |
| US5302274A (en) * | 1990-04-16 | 1994-04-12 | Minitech Co. | Electrochemical gas sensor cells using three dimensional sensing electrodes |
| CN102621205A (en) * | 2012-03-28 | 2012-08-01 | 华瑞科学仪器(上海)有限公司 | Hydrogen sulfide electrochemical transducer |
| CN104998636A (en) * | 2015-07-29 | 2015-10-28 | 贵州大学 | Synthetic method and application of PtRu binary metal nano-alloy catalyst |
| CN108872313A (en) * | 2018-06-21 | 2018-11-23 | 吉林大学 | Using Pt-Rh/C as current mode hydrogen sulfide sensor of sensitive electrode and preparation method thereof |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2004506181A (en) * | 2000-07-27 | 2004-02-26 | シティ テクノロジー リミテッド | Gas sensor |
| US20090184005A1 (en) * | 2004-10-25 | 2009-07-23 | Xueji Zhang | Sensor for Measurement of Hydrogen Sulfide |
| US20180266983A1 (en) * | 2015-08-24 | 2018-09-20 | Honeywell International Inc. | Electrochemical sensor |
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Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB2167192A (en) * | 1984-11-15 | 1986-05-21 | Atomic Energy Authority Uk | Gas sensor |
| US5173166A (en) * | 1990-04-16 | 1992-12-22 | Minitech Co. | Electrochemical gas sensor cells |
| US5302274A (en) * | 1990-04-16 | 1994-04-12 | Minitech Co. | Electrochemical gas sensor cells using three dimensional sensing electrodes |
| CN102621205A (en) * | 2012-03-28 | 2012-08-01 | 华瑞科学仪器(上海)有限公司 | Hydrogen sulfide electrochemical transducer |
| CN104998636A (en) * | 2015-07-29 | 2015-10-28 | 贵州大学 | Synthetic method and application of PtRu binary metal nano-alloy catalyst |
| CN108872313A (en) * | 2018-06-21 | 2018-11-23 | 吉林大学 | Using Pt-Rh/C as current mode hydrogen sulfide sensor of sensitive electrode and preparation method thereof |
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