CN114457356A - Method for preparing chlorine by photoelectrocatalysis - Google Patents
Method for preparing chlorine by photoelectrocatalysis Download PDFInfo
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- CN114457356A CN114457356A CN202210092919.2A CN202210092919A CN114457356A CN 114457356 A CN114457356 A CN 114457356A CN 202210092919 A CN202210092919 A CN 202210092919A CN 114457356 A CN114457356 A CN 114457356A
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- photoelectrocatalysis
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
- C25B1/01—Products
- C25B1/24—Halogens or compounds thereof
- C25B1/26—Chlorine; Compounds thereof
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
- C25B1/50—Processes
- C25B1/55—Photoelectrolysis
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
- C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
- C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
- C25B11/052—Electrodes comprising one or more electrocatalytic coatings on a substrate
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
- C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
- C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
- C25B11/073—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material
- C25B11/075—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of a single catalytic element or catalytic compound
- C25B11/077—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of a single catalytic element or catalytic compound the compound being a non-noble metal oxide
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Abstract
The invention relates to a method for preparing chlorine by photoelectrocatalysis, belonging to the technical field of chlorine preparation. Firstly, preparing a titanium dioxide film by a hydrothermal method, and then placing the titanium dioxide film in a muffle furnace for calcination to obtain conductive glass loaded with the titanium dioxide film; and then assembling the prepared conductive glass loaded with the titanium dioxide film, a reaction device and a collection device, applying bias voltage, and illuminating to obtain the device for preparing chlorine by photoelectrocatalysis. The invention introduces the light energy into the reaction device for preparing the chlorine, can fully utilize the light energy to realize the environment-friendly production of the chlorine, and utilizes the semiconductor material titanium dioxide as the photocatalyst to reduce the pollution to the environment.
Description
Technical Field
The invention belongs to the technical field of chlorine preparation, and particularly relates to a method for preparing chlorine through photoelectrocatalysis.
Background
In modern society, with the increasing consumption of fossil energy and the increasing environmental pollution, renewable energy is a focus of attention of researchers. At present, chlorine plays an important role in daily life, can be used for producing sodium hypochlorite, producing plastics and the like in industry, and can also be applied to a plurality of fields of sewage treatment, tap water disinfection, sterilization and insecticide, pharmacy and the like in breweries. The current methods for preparing chlorine mainly comprise methods of electrolyzing saturated salt water, oxidizing concentrated hydrochloric acid and the like, but the methods have the defects of energy waste, strong pollution, safety and the like. The preparation of chlorine by photoelectrocatalysis is a novel mode, and the method has the following remarkable advantages: (1) the method fully utilizes solar energy, widens the introduction ways of green energy sources such as solar energy and the like, reduces the input of extra energy sources, and reduces the cost for producing chlorine; (2) the chlorine production mode is safe and environment-friendly, the raw materials are cheap and easy to obtain, and meanwhile, the inorganic solution (saturated potassium chloride solution) is used as the electrolyte, so that the potential safety hazard caused by using concentrated hydrochloric acid as a reaction solution in the traditional method is avoided, and the method has a wide application prospect; (3) the semiconductor material is introduced into the experiment for producing chlorine by solar photoelectrocatalysis, so far, no relevant report appears. Therefore, the photoelectrocatalysis is considered to be a novel method for preparing chlorine with development prospect and innovation, and meanwhile, the method also provides important reference for further research of chlorine preparation and expansion of large-scale application field.
Disclosure of Invention
In order to solve the problems, the technical scheme adopted by the invention is as follows: a method for preparing chlorine by photoelectrocatalysis comprises the following steps:
1) preparing a titanium dioxide film by a hydrothermal method, and then placing the titanium dioxide film in a muffle furnace for calcining to obtain the conductive glass loaded with the titanium dioxide film;
2) assembling the conductive glass loaded with the titanium dioxide film prepared in the step 1), a reaction device and a collection device to obtain the device for preparing chlorine by photoelectrocatalysis.
Further, a method for preparing chlorine by photoelectrocatalysis, in the step 1), the method for preparing the conductive glass loaded with the titanium dioxide film comprises the following steps:
1) sequentially adding concentrated hydrochloric acid and titanium tetrachloride into 15mL of water, and stirring for 15min to obtain a solution A;
2) putting the cleaned conductive glass (FTO) into a reaction kettle, pouring the solution A prepared in the step 1) into the reaction kettle, immersing the conductive glass in the solution A, placing the solution A into an oven for heating reaction for 6 hours, taking out the conductive glass after cooling to 50 ℃, washing the conductive glass with deionized water, naturally drying the conductive glass, and then putting the conductive glass into a muffle furnace for calcining for 3 hours to obtain the conductive glass loaded with the titanium dioxide film.
Furthermore, the preparation method of the conductive glass loaded with the titanium dioxide film comprises the following steps of 1), according to the mass ratio, concentrated hydrochloric acid: titanium tetrachloride 27-30: 1.
Further, in the preparation method of the conductive glass loaded with the titanium dioxide film, in the step 2), the heating temperature in the oven is 165 ℃.
Furthermore, in the preparation method of the conductive glass loaded with the titanium dioxide film, in the step 2), the calcining temperature in the muffle furnace is 550 ℃.
Further, a method for preparing chlorine by photoelectrocatalysis, in the step 2), the preparation method of the device for preparing chlorine by photoelectrocatalysis comprises the following steps: the method comprises the steps of taking conductive glass loaded with a titanium dioxide film as a working electrode, Ag/AgCl as a reference electrode and a Pt wire as a counter electrode, under the condition of a three-electrode system, taking a potassium chloride solution as an electrolyte, taking a sodium hydroxide solution as an absorption liquid and a collection liquid, applying bias voltage, and giving illumination, thus completing the assembly of the photoelectrocatalysis chlorine gas preparation device.
Furthermore, the preparation method of the device for preparing chlorine by photoelectrocatalysis comprises the following steps: 34.5g of potassium chloride crystal is dissolved in 100mL of water, stirred for 15min and ultrasonically treated for 15min to fully dissolve the potassium chloride crystal.
Furthermore, the preparation method of the device for preparing chlorine by photoelectrocatalysis is comprises the following steps that: 0.04g of sodium hydroxide crystals was dissolved in 100mL of water and sonicated for 15min to dissolve them sufficiently.
In a further preparation method of the device for preparing chlorine by photoelectrocatalysis, the applied bias voltage is 1.13V.
The invention has the beneficial effects that:
1. the invention introduces the light energy into the chlorine gas production equipment, realizes the conversion from the solar energy to the electric energy, realizes the cooperative conversion of the solar energy, the electric energy and the chemical energy, and achieves the utilization effect of the solar energy.
2. The invention introduces the traditional semiconductor material titanium dioxide, reduces the energy consumption, uses the inorganic solution (saturated potassium chloride solution) as the reaction solution, and avoids the potential safety hazard caused by using concentrated hydrochloric acid as the reaction solution in the traditional method.
3. The invention adopts the titanium dioxide film as the photocatalyst, has excellent photocatalytic performance, obviously reduces the voltage for generating chlorine under illumination, improves the yield of chlorine, saves electric energy and widens the application range of green energy.
4. The invention introduces solar energy into a system for producing chlorine, further utilizes the existing renewable energy, prepares the chlorine under the condition of not consuming non-renewable energy such as fossil energy and the like, widens the utilization space of the renewable energy and realizes the green and environment-friendly production of the chlorine.
Drawings
FIG. 1 is a schematic structural diagram of a device for preparing chlorine by photoelectrocatalysis.
FIG. 2 is a schematic diagram of a device for preparing chlorine by photoelectrocatalysis.
Fig. 3 is an X-ray diffraction (XRD) spectrum of the titanium dioxide thin film.
Fig. 4 is a Linear Sweep Voltammetry (LSV) test chart of a titanium dioxide film (with water as the electrolyte).
Fig. 5 is a graph of Linear Sweep Voltammetry (LSV) measurements of a titanium dioxide film with a saturated potassium chloride solution as the electrolyte.
FIG. 6 is a graph showing the Linear Sweep Voltammetry (LSV) measurement of a titanium dioxide film using a potassium chloride solution containing 0.1M hydrochloric acid as an electrolyte.
FIG. 7 is a graph of current-time (i-t) measurements of titanium dioxide films.
FIG. 8 is an ion chromatogram of a 1000-fold diluted potassium chloride solution (before the electrolytic reaction).
Fig. 9 is an ion chromatogram of a potassium chloride solution (after electrolytic reaction) diluted 1000 times.
FIG. 10 is a graph showing the results of a chlorine ion meter test on a sodium hydroxide solution (before an electrolytic reaction).
FIG. 11 is a graph showing the results of a chlorine ion meter test on a sodium hydroxide solution (after an electrolytic reaction).
Detailed Description
Example 1A method for preparing chlorine by photoelectrocatalysis (I) a titanium dioxide film is loaded on FTO conductive glass
The preparation method comprises the following steps:
preparing a titanium dioxide film by a hydrothermal method, sequentially adding 16.5g of concentrated hydrochloric acid and 0.6g of titanium tetrachloride into 15mL of water, and stirring for 15min to uniformly mix the concentrated hydrochloric acid and the titanium tetrachloride to obtain a solution A; putting the cleaned conductive glass (FTO) into a reaction kettle, pouring the prepared solution A into the reaction kettle to immerse the conductive glass in the solution A, heating and reacting for 6 hours in a 165 ℃ oven, taking out the conductive glass after cooling to 50 ℃, washing the conductive glass with deionized water, naturally drying the conductive glass, and then putting the conductive glass into a muffle furnace to calcine for 3 hours at the calcining temperature of 550 ℃ to obtain the conductive glass loaded with the titanium dioxide film.
(II) preparing chlorine by photoelectrocatalysis
The preparation method comprises the following steps:
an electrochemical workstation is utilized, conductive glass loaded with a titanium dioxide film is used as a working electrode, Ag/AgCl is used as a reference electrode, Pt wires are used as a counter electrode, saturated potassium chloride solution is used as electrolyte and is respectively inserted into rubber plugs with proper pore diameters, the rubber plugs are placed on a quartz beaker of the saturated potassium chloride solution, 100mL of 0.01M sodium hydroxide solution is prepared and is evenly filled into two glass bottles, one bottle is used as collecting liquid, the other bottle is used as absorbing liquid, a reaction device and a collecting device are communicated through a conduit, a ventilating position is sealed through plasticine, 1.13V bias voltage is applied, irradiation is carried out for 1.5h under simulated sunlight (a xenon lamp is used as a light source), and the generated chlorine can be absorbed and collected in the sodium hydroxide solution to ensure that the titanium dioxide film can be sufficiently irradiated by the simulated sunlight (AM 1.5). The structural schematic diagram of the device for preparing chlorine by photoelectrocatalysis is shown in figure 1, and the physical diagram is shown in figure 2.
(III) testing and calculating
1) XRD test
The characteristic spectrum of the titanium dioxide film is shown in figure 3 by XRD test, and as can be seen from figure 3, the sample shows a more obvious titanium dioxide characteristic diffraction peak with a sharp peak type, which indicates that the obtained product is the titanium dioxide semiconductor film with higher crystallinity.
2) Linear Sweep Voltammetry (LSV) testing
Water, a saturated potassium chloride solution and a potassium chloride solution containing 0.1M hydrochloric acid are respectively selected as electrolytes to verify the photocatalytic activity of the titanium dioxide film, different reaction systems are respectively subjected to Linear Sweep Voltammetry (LSV) tests, as can be seen from figures 4 to 6, the titanium dioxide film is used as a photocatalyst in three different electrolytes, the oxygen generation voltage under the illumination condition is lower than the oxygen generation voltage under the dark condition, and the chlorine generation voltage under the illumination condition is also lower than the chlorine generation voltage under the dark condition; as shown in FIG. 5, the chlorine generating voltage under light was reduced to 0.2V, which was 1.8V compared to about 2V under dark conditions, demonstrating that the titanium dioxide film has excellent photocatalytic activity.
3) Current-time (i-t) test
From the results of the i-t test in fig. 7, the total amount of charge involved in the reaction in the circuit was 10.45C.
4) Ion chromatography for measuring chloride ion
The potassium chloride solutions before and after the electrolysis were diluted 1000 times and detected by ion chromatography, and it was found from the data in fig. 8 and 9 that the peak area of chloride ions in the potassium chloride electrolyte decreased from 167.269 before the electrolysis to 164.279 after the electrolysis, indicating that some chloride ions were reduced by oxidation.
5) Chloride ion meter for measuring chloride ion
The chlorine ion concentrations in the sodium hydroxide solution before and after the electrolytic reaction were measured by the chlorine ion meter, and as is clear from the data in FIGS. 10 and 11, the chlorine ion concentration before the reaction was 10 because the measurement value before the reaction was 5.62 and the measurement value after the reaction was 5.26 in the sodium hydroxide solution-5.62＝2.3988×10-6mol/L, the concentration of chloride ion after reaction is 10-5.26＝5.495×10-6mol/L, the total volume of the sodium hydroxide solution is 0.1L, so that the concentration of chloride ions in the sodium hydroxide solution is increased, and the number of electrons participating in the reaction is as follows: (5.495X 10)-6-2.3988×10-6)×2×0.1＝6.1924×10-7And (mol). The method shows that part of chloride ions in the potassium chloride electrolyte are subjected to oxidation reaction to generate chlorine, and the chlorine then enters the sodium hydroxide solution through the guide pipe and reacts with the sodium hydroxide solution to increase the concentration of the chloride ions.
6) Calculation of chlorine production efficiency
As can be seen from the data in fig. 7, the total amount of charge involved in the reaction in the circuit is 10.45C, which is converted to: the total electron quantity in the circuit is 1.085X 10-4mol, from 5) it is known that the concentration of chloride ions in the sodium hydroxide solution is increased and the number of electrons participating in the reaction is 6.1924X 10-7And (mol). The calculation of the chlorine production efficiency is therefore as follows:
namely, the chlorine production efficiency in the total system was 0.57%.
Claims (9)
1. The method for preparing chlorine by photoelectrocatalysis is characterized by comprising the following steps:
1) preparing a titanium dioxide film by a hydrothermal method, and then placing the titanium dioxide film in a muffle furnace for calcining to obtain the conductive glass loaded with the titanium dioxide film;
2) assembling the titanium dioxide film-loaded conductive glass prepared in the step 1), a reaction device and a collection device to obtain the device for preparing chlorine through photoelectrocatalysis.
2. The method for preparing chlorine gas through photoelectrocatalysis according to claim 1, wherein in the step 1), the preparation method of the conductive glass loaded with the titanium dioxide thin film comprises the following steps:
1) sequentially adding concentrated hydrochloric acid and titanium tetrachloride into 15mL of water, and stirring for 15min to obtain a solution A;
2) putting the cleaned conductive glass (FTO) into a reaction kettle, pouring the solution A prepared in the step 1) into the reaction kettle, immersing the conductive glass in the solution A, placing the solution A into an oven for heating reaction for 6 hours, taking out the conductive glass after cooling to 50 ℃, washing the conductive glass with deionized water, naturally drying the conductive glass, and then putting the conductive glass into a muffle furnace for calcining for 3 hours to obtain the conductive glass loaded with the titanium dioxide film.
3. The method for preparing chlorine by photoelectrocatalysis according to claim 2, characterized in that: in the step 1), according to the mass ratio, concentrated hydrochloric acid: titanium tetrachloride 27-30: 1.
4. The method for preparing chlorine by photoelectrocatalysis according to claim 2, characterized in that: in the step 2), the heating temperature in the oven is 165 ℃.
5. The method for preparing chlorine by photoelectrocatalysis according to claim 2, characterized in that: in the step 2), the calcining temperature in the muffle furnace is 550 ℃.
6. The method for preparing chlorine by photoelectrocatalysis as claimed in claim 1, wherein in the step 2), the preparation method of the device for preparing chlorine by photoelectrocatalysis is comprises the following steps: the method comprises the steps of taking conductive glass loaded with a titanium dioxide film as a working electrode, Ag/AgCl as a reference electrode and a Pt wire as a counter electrode, under the condition of a three-electrode system, taking a potassium chloride solution as an electrolyte, taking a sodium hydroxide solution as an absorption liquid and a collection liquid, applying bias voltage, and giving illumination, thus completing the assembly of the photoelectrocatalysis chlorine preparation device.
7. The method for preparing chlorine by photoelectrocatalysis according to claim 6, characterized in that: the potassium chloride solution is a saturated potassium chloride solution, and the preparation method comprises the following steps: 34.5g of potassium chloride crystal is dissolved in 100mL of water, stirred for 15min and ultrasonically treated for 15min to fully dissolve the potassium chloride crystal.
8. The method for preparing chlorine by photoelectrocatalysis according to claim 6, characterized in that: the sodium hydroxide solution is 0.01M sodium hydroxide solution, and the preparation method comprises the following steps: 0.04g of sodium hydroxide crystals was dissolved in 100mL of water and sonicated for 15min to dissolve them sufficiently.
9. The method of claim 6, wherein the bias voltage is 1.13V.
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Citations (5)
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| CN102254697A (en) * | 2011-04-25 | 2011-11-23 | 宁波大学 | Titanium dioxide light anode, and preparation method and use thereof |
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| CN105931848A (en) * | 2016-05-23 | 2016-09-07 | 吉林大学 | Cu3BiS3 sensitized TiO2 oxide film in-situ and hydrothermally grown on FTO, preparation method and application thereof |
| CN112536032A (en) * | 2020-12-04 | 2021-03-23 | 浙江师范大学 | High-temperature-resistant sintering catalyst for preparing chlorine by oxidizing hydrogen chloride and preparation method thereof |
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- 2022-01-26 CN CN202210092919.2A patent/CN114457356B/en active Active
Patent Citations (5)
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| KR20120119270A (en) * | 2011-04-21 | 2012-10-31 | 한국에너지기술연구원 | Apparatus and method for photoelectrochemical hydrogen production using by preparation of electrodeposited pt on tio2 natubular electrode as cathode, natural seawater and concentrated seawater electrolytes obtained from membrane process |
| CN102254697A (en) * | 2011-04-25 | 2011-11-23 | 宁波大学 | Titanium dioxide light anode, and preparation method and use thereof |
| CN104658761A (en) * | 2015-02-26 | 2015-05-27 | 江汉大学 | Method for preparing dye-sensitized solar cell nano-TiO2 membrane photo-anode with membrane reaction method |
| CN105931848A (en) * | 2016-05-23 | 2016-09-07 | 吉林大学 | Cu3BiS3 sensitized TiO2 oxide film in-situ and hydrothermally grown on FTO, preparation method and application thereof |
| CN112536032A (en) * | 2020-12-04 | 2021-03-23 | 浙江师范大学 | High-temperature-resistant sintering catalyst for preparing chlorine by oxidizing hydrogen chloride and preparation method thereof |
Non-Patent Citations (1)
| Title |
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| 黄慧萍等: "金属氧化物催化氧化氯化氢制氯气的研究" * |
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