CN113416977B - KRu 4 O 8 Nanorod material, preparation method and application thereof - Google Patents
KRu 4 O 8 Nanorod material, preparation method and application thereof Download PDFInfo
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Abstract
The invention provides KRu 4 O 8 Nanorod material with rim [001]Directionally grown barium manganese ore structure. The application also provides KRu 4 O 8 A method for preparing a nanorod material, comprising the steps of: mixing a ruthenium chloride aqueous solution and a potassium hydroxide aqueous solution, and reacting to obtain a precipitate; calcining the precipitate at high temperature to obtain KRu 4 O 8 A nanorod material. The application also provides KRu 4 O 8 The application of the nano-rod material in the reaction of synthesizing 1, 2-propylene glycol by electrochemical oxidation of propylene. KRu in the present application 4 O 8 The introduction of the MnBa ore structure and the large-radius potassium atom of the nano rod material improves the catalytic activity and selectivity of synthesizing 1, 2-propylene glycol by electrochemical propylene oxide.
Description
Technical Field
The invention relates to the technical field of catalysts, and particularly relates to KRu 4 O 8 A nanorod material, a preparation method and application thereof.
Background
1, 2-propylene glycol is a chemical with higher added value, can be applied to the manufacture of products such as paint, liquid detergent, cosmetics, essence, food, personal care products, tobacco humectant and the like, and is mainly used as an antifreezing coolant and a deicing agent, and used as a raw material for polyester resin synthesis for fiber production and medical production.
Industrial processes for the production of 1, 2-propanediol, such as propylene oxide hydration and glycerol hydrogenolysis, require multiple steps and are energy intensive. The reduction of fossil fuel resources, the increase of environmental problems, and the global impact on energy, fuel, and chemical demand have greatly increased the drive for the research of electrochemical synthesis. The method for processing the propylene to produce the high-value product 1, 2-propylene glycol by using the environment-friendly electrochemical method to replace the traditional propylene high-temperature high-pressure oxidation rehydration process is a very valuable research direction. Several previous reports have investigated the results of direct electrochemical oxidation of propylene, however most of the earlier studies used metallic palladium electrocatalysts which did not show high selectivity to economically valuable 1, 2-propanediol. On the other hand, ruthenium-based materials have been widely used for the electro-oxidation of small organic molecules such as methanol and glycerol. According to previous literature reports, ruthenium-based materials have not been applied to the electrooxidation of propylene.
Disclosure of Invention
The invention aims to provide KRu 4 O 8 The nano rod material provided by the application is applied to electrochemical oxidation of propylene to synthesize 1, 2-propylene glycol, and has high selectivity, activity and catalytic stability.
In view of the above, the present application provides a KRu 4 O 8 A nanorod material having a rim [001]Directionally grown barium manganese ore structure.
Preferably, the KRu is 4 O 8 The length of the nano rod material is 150-300 nm, and the diameter is 30-60 nm.
The application also provides the KRu 4 O 8 The preparation method of the nano rod material comprises the following steps:
mixing a ruthenium chloride aqueous solution and a potassium hydroxide aqueous solution, and reacting to obtain a precipitate;
calcining the precipitate at high temperature to obtain KRu 4 O 8 A nanorod material.
Preferably, the concentration of the ruthenium chloride aqueous solution is less than or equal to 0.5mol/L, and the concentration of the potassium hydroxide aqueous solution is more than or equal to 5mol/L.
Preferably, the mixing time is 20 to 60min.
Preferably, the calcination further comprises drying, and the drying temperature is 80-120 ℃.
Preferably, the calcining temperature is 500-1000 ℃ and the time is 2-8 h.
Preferably, the calcination is carried out in argon and oxygen in a volume ratio of 3.
The application also provides the KRu 4 O 8 Nano rod material or KRu prepared by using preparation method 4 O 8 The application of the nano-rod material in synthesizing 1, 2-propylene glycol by electrochemical oxidation of propylene.
The application provides a KRu 4 O 8 A nanorod material having a rim [001]Directionally grown barium manganese ore structure; due to KRu 4 O 8 The MnBa ore structure of the nano-rod material forms a structural form with K atoms on the surface, and the introduction of the large-radius K atoms causes structural phase deformation, thereby regulating and controlling the adsorption strength of a propylene intermediate on the surface of the nano-rod material, improving the slow kinetics of the partial oxidation process of propylene, and improving KRu 4 O 8 The nano rod material has catalytic activity, selectivity and catalytic stability in the application of synthesizing 1, 2-propylene glycol by electrochemical oxidation of propylene.
Drawings
FIG. 1 shows a KRu of one-dimensional MnBaite structure prepared in example 1 of the present invention 4 O 8 Scanning electron microscope pictures of nanorod catalysts;
FIG. 2 shows the structure KRu of one-dimensional MnBaite prepared in example 1 of the present invention 4 O 8 Transmission electron microscope picture of nanorod catalyst;
FIG. 3 shows KRu in one-dimensional MnBazite structure prepared in example 1 of the present invention 4 O 8 High resolution transmission electron microscope pictures of nanorod catalysts;
FIG. 4 shows a KRu with one-dimensional MnBazite structure prepared in example 1 of the present invention 4 O 8 The X-ray diffraction pattern of the nanorod catalyst;
FIG. 5 shows a KRu with one-dimensional MnBazite structure prepared in example 1 of the present invention 4 O 8 Nanorod catalyst and commercial RuO 2 An X-ray photoelectron spectrum of the catalyst;
FIG. 6 shows a KRu with one-dimensional MnBazite structure prepared in example 1 of the present invention 4 O 8 Nanorod catalyst and commercial RuO 2 An X-ray absorption near-edge spectrum of the catalyst;
FIG. 7 shows a KRu with one-dimensional MnBazite structure prepared in example 3 of the present invention 4 O 8 Nanorod catalyst and commercial RuO 2 The effective current density of the catalyst under different overpotentials is shown;
FIG. 8 shows KRu in one-dimensional MnBaite structure prepared in example 3 of this invention 4 O 8 Faradaic efficiency of producing 1, 2-propylene glycol by the nanorod catalyst under different overpotentials;
FIG. 9 shows KRu in one-dimensional MnBaite structure prepared in example 4 of this invention 4 O 8 Graph showing the change of Faraday efficiency of 1, 2-propanediol produced by the nanorod catalyst under the overpotential of 1.5V relative to a standard hydrogen electrode along with time.
Detailed Description
For a further understanding of the invention, reference will now be made to the preferred embodiments of the invention by way of example, and it is to be understood that the description is intended to further illustrate features and advantages of the invention, and not to limit the scope of the claims.
In view of the current situation of propylene electro-oxidation, the application provides a KRu with a one-dimensional manganite structure 4 O 8 The nano rod material has high selectivity and activity and good catalytic stability in the reaction of synthesizing 1, 2-propylene glycol by electrochemically oxidizing propylene. Specifically, the embodiment of the invention discloses KRu 4 O 8 A nanorod material having a rim [001]Directionally grown barium manganese ore structure.
In the present application, the KRu 4 O 8 The length of the nano rod material is 150-300 nm, and the diameter is 30-60 nm.
The application also provides the KRu 4 O 8 The preparation method of the nano rod material comprises the following steps:
mixing a ruthenium chloride aqueous solution and a potassium hydroxide aqueous solution, and reacting to obtain a precipitate;
calcining the precipitate at high temperature to obtain KRu 4 O 8 A nanorod material.
In the preparation of KRu 4 O 8 In the process of preparing the nano rod material, firstly, mixing a ruthenium chloride aqueous solution and a potassium hydroxide aqueous solution, and reacting to obtain a precipitate; in this process, potassium hydroxide reacts with ruthenium chloride to give a ruthenium hydroxide precipitate, which adsorbs a portion of the KOH in solution to form a precipitate. In the process, the concentration of the ruthenium chloride aqueous solution is less than or equal to 0.5mol/L, and the concentration of the potassium hydroxide aqueous solution isNot less than 5mol/L; in a specific embodiment, the concentration of the ruthenium chloride aqueous solution is 0.5mol/L, and the concentration of the potassium hydroxide aqueous solution is 5mol/L. The concentrations of the potassium hydroxide aqueous solution and the ruthenium chloride aqueous solution can affect the purity, the length and the thickness of the nanorod phase; the aqueous solution of potassium hydroxide is in excess and has a concentration of 5mol/L or more, otherwise RuO occurs 2 Miscellaneous phase; likewise, the concentration of the aqueous solution of ruthenium chloride is less than or equal to 0.5mol/L, otherwise RuO will occur 2 Miscellaneous phase, reduction of RuCl 3 The rod-shaped material is shortened by the feeding amount. The mixing needs to be continuously stirred for 20-60 min to allow the reaction to fully proceed. The application then dries the precipitate at 80-120 ℃.
The application finally high temperature calcination of the precipitate to obtain KRu 4 O 8 A nanorod material. In the calcining process, ruthenium hydroxide and potassium hydroxide react with oxygen to obtain KRu 4 O 8 (ii) a Controlling the concentration of the raw materials and the reaction conditions to obtain KRu 4 O 8 A nanorod material. In the calcining process, the calcining is carried out in a mixed gas of argon and oxygen in a volume ratio of 3.
The application also provides the KRu 4 O 8 The application of the nano-rod material in the electrochemical oxidation of propylene to synthesize 1, 2-propylene glycol.
In a specific embodiment of the present application, the process of electrochemical oxidation is:
5 mg of KRu with one-dimensional manganite structure 4 O 8 Dispersing the nanorod catalyst, 5 mg of activated carbon and 25 microliters of 5% mass fraction Nafion solution in 475 milliliters of ethanol, and performing ultrasonic mixing for at least 45 minutes to obtain a uniform catalyst ink; then spraying catalyst ink on the carbon-based fiber gas diffusion layer, wherein the loading amount of the catalyst is kept to be 1 mg/square centimeter; the gas diffusion layer is used as a working electrode, the calomel electrode is used as a reference electrode, and the platinum wire is used as a counter electrode. The electrochemical reaction for synthesizing 1, 2-propylene glycol by propylene oxide is carried out in a three-channel flow cell, and electrolyteThe electrolyte containing 0.5mol/L sulfuric acid is applied with overpotential and detected current density through an electrochemical workstation.
Commercial RuO 2 Preparation of electrode and KRu 4 O 8 The electrode preparation remains the same.
With commercial RuO 2 Comparing the nano-catalyst, and in the reaction of synthesizing 1, 2-propylene glycol by electrochemical propylene oxide, under the overpotential of 1.5V relative to the standard hydrogen electrode, the KRu with the one-dimensional manganese barium ore structure 4 O 8 The nanorod catalyst has a current density of about 18.3 mA/cm, faradaic efficiency of 1, 2-propanediol production up to 62%, and an effective current density of 11.3 mA/cm, as compared to commercial RuO 2 The nano-catalyst does not show the activity of synthesizing 1, 2-propylene glycol by the electro-oxidation of propylene. One-dimensional manganite structure KRu used in the invention 4 O 8 Compared with other catalytic materials, the nanorod catalyst is easy to synthesize in a large scale and low in cost. In the catalytic reaction, the catalyst used in the invention has high selectivity and good stability.
For further understanding of the present invention, the following examples are given to KRu provided by the present invention 4 O 8 The nanorod materials, methods of making and uses thereof are described in detail, and the scope of the present invention is not limited by the following examples.
Example 1
The invention provides KRu with a one-dimensional manganite structure 4 O 8 The nano-rod catalyst has a length of 150-300 nm, a diameter of about 50 nm, and a length of [001 ]]Directional growth; the synthesis method comprises the following steps:
0.5 ml of an aqueous ruthenium chloride solution (0.5 mol/l) was added to 50 ml of an aqueous potassium hydroxide solution (5 mol/l) and stirring was continued for 30 minutes, the precipitate becoming thicker with increasing time; then, the precipitate was filtered and kept in an oven at 100 ℃ overnight; after milling, the precipitated powder was calcined at 750 ℃ for 4 hours in a mixed gas of argon and oxygen (3; the final product was washed with deionized water and centrifuged 5 times to remove excess ions and obtain KRu 4 O 8 A nanorod material.
KRu with one-dimensional manganite structure 4 O 8 The scanning electron microscope picture of the nanorod catalyst is shown in figure 1, the transmission electron microscope picture is shown in figure 2, the high-resolution transmission electron microscope picture is shown in figure 3, the X-ray diffraction spectrum is shown in figure 4, the X-ray photoelectron spectrum is shown in figure 5, and the X-ray absorption near-edge spectrum is shown in figure 6.
Example 2
KRu with one-dimensional manganite structure 4 O 8 The nano-rod catalyst is used as an electro-catalyst of an active ingredient and the electrochemical propylene oxide test condition.
5 mg of KRu with one-dimensional manganite structure 4 O 8 A nano rod material, 5 mg of activated carbon, 500. Mu.l of ethanol, 475. Mu.l of water and 25. Mu.l of Nafion solution (mass fraction: 5%) were ultrasonically mixed for at least 45 minutes to prepare a catalyst ink; then spraying catalyst ink on the carbon-based fiber gas diffusion layer, wherein the loading capacity of the catalyst is kept at 1 mg/square centimeter; the gas diffusion layer is used as a working electrode, the calomel electrode is used as a reference electrode, and the platinum net is used as a counter electrode; the electrochemical propylene oxide reaction electrolyte is 0.5mol/L sulfuric acid solution, the catalytic reaction is carried out in a three-channel flow cell with the channel size of 2 cm multiplied by 0.5 cm multiplied by 0.15 cm, and the gas flow flowing into the flow cell is controlled at 10 standard milliliters/minute through a Brooks GF40 mass flow controller. The flow rates of the catholyte and anolyte were controlled by peristaltic pumps, with the flow rate of the catholyte ranging from 0.1 to 1 ml/min, depending on the current density (low flow rates were used at low current densities to allow sufficient accumulation of liquid product); the anode liquid flow rate was fixed at 5 ml/min. The cathode and anode were separated by a hydroxide exchange membrane (FAA-3. The back pressure of the gas in the flow cell was controlled to atmospheric pressure using a back pressure controller (Cole-Parmer).
Example 3
KRu with one-dimensional manganite structure 4 O 8 And (3) testing the current density and the product selectivity of the nanorod catalyst in a test for synthesizing 1, 2-propylene glycol by electrochemical oxidation of propylene.
Under the reaction conditions of example 2, a potentiostatic test was employed. Setting up a phaseThe overpotential of the standard hydrogen electrode is 1.4V, and the constant potential is tested for 10 minutes; the concentration of the 1, 2-propylene glycol generated after the reaction is finished is detected and calculated by a nuclear magnetic resonance hydrogen spectrum. After the test was completed, the overpotential was changed to 1.45v,1.5v,1.55v,1.6v,1.65v,1.7v, and the test was performed by the same procedure, respectively. KRu in one-dimensional manganite structure 4 O 8 The current density of the nanorod catalyst under the overpotentials is shown in figure 7, and the faradaic efficiency of producing 1, 2-propylene glycol under different potentials is shown in figure 8; FIG. 7 shows the signal at 0.5M H 2 SO 4 The propylene electrooxidation polarization curve recorded in the electrolyte; the current density increased with increasing applied voltage, indicating that the mass transport limitation of propylene was not significant; using commercial RuO 2 With KRu 4 O 8 Nanorod contrast, commercial RuO 2 Shows much lower current density at the same applied potential under a propylene atmosphere. As can be seen from FIG. 8, the Faraday efficiency of 1, 2-propanediol first increased and then decreased with increasing potential, reaching a peak of 62% at 1.5V over-potential relative to the standard hydrogen electrode; the total faradaic efficiency of propylene electrooxidation reaches the maximum value of 71 percent when the overpotential is 1.5V relative to the standard hydrogen electrode; further increasing the applied potential to greater than 1.5V over the standard hydrogen electrode significantly reduced the selectivity to 1, 2-propanediol while increasing the selectivity to formic and acetic acids due to excessive oxidation of propylene.
Example 4
Under the condition that the overpotential relative to a standard hydrogen electrode is 1.5V, the KRu with the one-dimensional manganite structure 4 O 8 And (3) testing the stability of the nanorod catalyst in the synthesis of 1, 2-propylene glycol by electrochemical oxidation of propylene.
Under the reaction conditions of example 2, a potentiostatic test was employed. Setting the overpotential of the standard hydrogen electrode to be 1.5V, and carrying out constant potential test for 8 hours. During the reaction, the liquid product was taken every 1 hour, and the 1, 2-propanediol concentration was calculated by measuring the NMR spectrum. KRu with one-dimensional manganite structure 4 O 8 The time-dependent change graphs of the current density of the nanorod catalyst at the potential and the faradaic efficiency of producing 1, 2-propanediol are shown in FIG. 9; as can be seen from FIG. 9, the stability test was carried out for 8 hoursPeriod, KRu 4 O 8 The current density of the nanorods and the faradaic efficiency of producing 1, 2-propanediol remained stable.
The above description of the embodiments is only intended to facilitate the understanding of the method of the invention and its core idea. It should be noted that, for those skilled in the art, it is possible to make various improvements and modifications to the present invention without departing from the principle of the present invention, and those improvements and modifications also fall within the scope of the claims of the present invention.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (6)
1. KRu 4 O 8 The preparation method of the nano rod material is characterized by comprising the following steps of:
mixing a ruthenium chloride aqueous solution and a potassium hydroxide aqueous solution, and reacting to obtain a precipitate;
calcining the precipitate at high temperature to obtain KRu 4 O 8 A nanorod material;
the concentration of the ruthenium chloride aqueous solution is less than or equal to 0.5mol/L, and the concentration of the potassium hydroxide aqueous solution is more than or equal to 5mol/L;
the calcination is carried out in argon and oxygen in a volume ratio of 3;
the KRu 4 O 8 Nanorod material with rim [001]Directionally grown barium manganese ore structure.
2. The method of claim 1, wherein the KRu is prepared by a known method 4 O 8 The length of the nano rod material is 150-300 nm, and the diameter is 30-60 nm.
3. The method of claim 2, wherein the mixing time is 20 to 60min.
4. The method according to claim 2, further comprising drying the calcined product at a temperature of 80 to 120 ℃.
5. The method according to claim 2, wherein the calcination is carried out at a temperature of 500 to 1000 ℃ for 2 to 8 hours.
6. KRu produced by the production method according to any one of claims 1 to 5 4 O 8 The application of the nano-rod material in synthesizing 1, 2-propylene glycol by electrochemical oxidation of propylene.
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| US5302257A (en) * | 1992-02-21 | 1994-04-12 | Sepracor, Inc. | Electrocatalytic asymmetric dihydroxylation of olefinic compounds |
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| JPS55161080A (en) * | 1979-06-01 | 1980-12-15 | Toyo Soda Mfg Co Ltd | Manufacture of glycols |
| KR100198976B1 (en) * | 1997-03-31 | 1999-06-15 | 이종훈 | Method of removing ruthenium compounds in industrial waste gas |
| DE19841872A1 (en) * | 1998-09-14 | 2000-03-16 | Creavis Tech & Innovation Gmbh | Electrocatalytic selective oxidation of hydrocarbons |
| CN106984305B (en) * | 2017-05-05 | 2019-04-26 | 哈尔滨工业大学 | A kind of high-efficient electrolytic water catalyst HRu4O8Micron bar and preparation method thereof |
| CN109487298B (en) * | 2018-12-07 | 2020-01-07 | 厦门大学 | Method for preparing ethylene glycol by electrocatalysis of formaldehyde |
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