CN221663030U - A device for preparing anode catalyst used in organic matter oxidation - Google Patents

A device for preparing anode catalyst used in organic matter oxidation Download PDF

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CN221663030U
CN221663030U CN202323528686.5U CN202323528686U CN221663030U CN 221663030 U CN221663030 U CN 221663030U CN 202323528686 U CN202323528686 U CN 202323528686U CN 221663030 U CN221663030 U CN 221663030U
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exchange membrane
proton exchange
reactor
oxidation
anode catalyst
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邵明飞
周华
李洋
栗振华
段雪
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Quzhou Resource Chemical Innovation Research Institute
Beijing University of Chemical Technology
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Quzhou Resource Chemical Innovation Research Institute
Beijing University of Chemical Technology
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Abstract

本实用新型公开了一种应用于有机物氧化中的阳极催化剂的制备装置,包括反应机构和电解机构,所述反应机构包括加热装置、放置于加热装置的加热腔内的反应器以及置于反应器上方的层析柱;所述电解机构包括质子交换膜电解槽以及为其供能的直流电源;质子交换膜电解槽的进料口与反应器出口通过输出管连接,质子交换膜电解槽的出料口与层析柱进气口通过输入管连接;导电基底放置于层析柱内。本实用新型可用于制备电解水阳极氧化有机物和电催化析氧反应耦合阴极制氢的催化剂,制备装置结构简单,可以实现温和条件下快速制备大面积催化剂,且装置清洁环保,利用装置合成的催化剂性能优异。

The utility model discloses a preparation device for anode catalysts used in organic oxidation, including a reaction mechanism and an electrolysis mechanism, wherein the reaction mechanism includes a heating device, a reactor placed in a heating chamber of the heating device, and a chromatography column placed above the reactor; the electrolysis mechanism includes a proton exchange membrane electrolyzer and a DC power supply for powering it; the feed port of the proton exchange membrane electrolyzer is connected to the reactor outlet through an output pipe, and the discharge port of the proton exchange membrane electrolyzer is connected to the gas inlet of the chromatography column through an input pipe; and a conductive substrate is placed in the chromatography column. The utility model can be used to prepare catalysts for electrolytic water anode oxidation of organic matter and electrocatalytic oxygen evolution reaction coupled cathode hydrogen production. The preparation device has a simple structure, can realize rapid preparation of large-area catalysts under mild conditions, and the device is clean and environmentally friendly, and the catalyst synthesized by the device has excellent performance.

Description

一种应用于有机物氧化中的阳极催化剂的制备装置A device for preparing anode catalyst used in organic matter oxidation

技术领域Technical Field

本实用新型属于催化剂合成装置,具体涉及一种应用于有机物氧化中的阳极催化剂的制备装置。The utility model belongs to a catalyst synthesis device, in particular to a preparation device of an anode catalyst used in the oxidation of organic matter.

背景技术Background Art

氢能由于具有燃烧热值高,清洁无污染等优点收到研究人员的广泛关注。目前氢气的主要来源依然是化石燃料制氢,这种途径虽然工艺成熟,具备较强的规模效应,但化石燃料制氢会排放大量二氧化碳,破坏环境,这与当前保护环境,节能减排的观念背道而驰。因此,寻找一种新型制氢途径就迫在眉睫。近些年电解水制氢由于其具有清洁环保,制取氢气纯度较高等优点受到研究人员的广泛关注。然而电解水制氢的过电势较高,成本较高等缺点制约了其工业应用前景。针对这些问题,使用性能优异的催化剂降低其过电势,提效降本是未来资源有效利用的一种重要实现方案。Hydrogen energy has received extensive attention from researchers due to its advantages such as high combustion calorific value and cleanliness. At present, the main source of hydrogen is still fossil fuel hydrogen production. Although this method has mature technology and strong scale effect, fossil fuel hydrogen production will emit a large amount of carbon dioxide and damage the environment, which runs counter to the current concept of protecting the environment, energy conservation and emission reduction. Therefore, it is urgent to find a new hydrogen production method. In recent years, hydrogen production by water electrolysis has attracted extensive attention from researchers due to its advantages such as cleanliness, environmental protection, and high purity of hydrogen production. However, the high overpotential and high cost of hydrogen production by water electrolysis restrict its industrial application prospects. In response to these problems, using catalysts with excellent performance to reduce its overpotential and improve efficiency and reduce costs is an important solution for the effective utilization of resources in the future.

在之前的研究中,贵金属通常被认为是性能优异的电解水氧化耦合制氢催化剂,但由于其价格较高,原料较少等缺点制约了其发展。近些年的研究主要集中在降低贵金属负载量或者使用廉价且储量巨大的过渡金属来研发新型电解水氧化耦合制氢催化剂。传统催化剂合成方法和装置,例如水热合成法及其装置,具有合成条件要求较高,无法大面积制备等缺点,这制约了催化剂研究的进一步发展。In previous studies, precious metals are generally considered to be excellent catalysts for the coupled hydrogen production from water electrolysis and oxidation, but their development is restricted by their high prices and limited raw materials. Research in recent years has mainly focused on reducing the loading of precious metals or using cheap and abundant transition metals to develop new catalysts for the coupled hydrogen production from water electrolysis and oxidation. Traditional catalyst synthesis methods and devices, such as hydrothermal synthesis and its devices, have the disadvantages of high requirements for synthesis conditions and the inability to prepare on a large scale, which restricts the further development of catalyst research.

实用新型内容Utility Model Content

本实用新型是为了克服现有技术中存在的缺点而提出的,其目的是提供一种应用于有机物氧化中的阳极催化剂的制备装置。The utility model is proposed to overcome the shortcomings in the prior art, and its purpose is to provide a device for preparing an anode catalyst used in the oxidation of organic matter.

本实用新型是通过以下技术方案实现的:The utility model is realized by the following technical solutions:

一种应用于有机物氧化中的阳极催化剂的制备装置,包括反应机构和电解机构,所述反应机构包括加热装置、放置于加热装置的加热腔内的反应器以及置于反应器上方的层析柱;所述电解机构包括质子交换膜电解槽以及为其供能的直流电源;质子交换膜电解槽的进料口与反应器出口通过输出管连接,质子交换膜电解槽的出料口与层析柱进气口通过输入管连接;导电基底放置于层析柱内,且位于隔板上方。A device for preparing an anode catalyst used in the oxidation of organic matter comprises a reaction mechanism and an electrolysis mechanism, wherein the reaction mechanism comprises a heating device, a reactor placed in a heating chamber of the heating device, and a chromatography column placed above the reactor; the electrolysis mechanism comprises a proton exchange membrane electrolyzer and a DC power supply for supplying energy thereto; the feed inlet of the proton exchange membrane electrolyzer is connected to the reactor outlet via an output pipe, and the discharge port of the proton exchange membrane electrolyzer is connected to the gas inlet of the chromatography column via an input pipe; and a conductive substrate is placed in the chromatography column and is located above a partition.

在上述技术方案中,所述输出管上设置泵,输出管一端伸入反应器内部,且位于液面上方,输出管与反应器的出口之间通过密封件密封。In the above technical solution, a pump is arranged on the output pipe, one end of the output pipe extends into the reactor and is located above the liquid surface, and the output pipe and the outlet of the reactor are sealed by a sealing member.

在上述技术方案中,所述层析柱顶端敞口,且设置可拆卸密封盖。In the above technical solution, the top of the chromatography column is open and is provided with a detachable sealing cover.

在上述技术方案中,所述层析柱进气口设置于隔板下方。In the above technical solution, the gas inlet of the chromatography column is arranged below the partition.

在上述技术方案中,所述层析柱下端插入反应器内,且两者之间密封处理。In the above technical solution, the lower end of the chromatography column is inserted into the reactor, and the two are sealed.

在上述技术方案中,所述直流电源正极通过电线连接质子交换膜电解槽的阳极板,其负极通过电线连接质子交换膜电解槽的阴极板。In the above technical solution, the positive electrode of the DC power supply is connected to the anode plate of the proton exchange membrane electrolyzer through an electric wire, and the negative electrode thereof is connected to the cathode plate of the proton exchange membrane electrolyzer through an electric wire.

在上述技术方案中,所述质子交换膜电解槽的进料口和出料口均设置于阳极板侧。In the above technical solution, the feed inlet and the discharge outlet of the proton exchange membrane electrolyzer are both arranged on the anode plate side.

在上述技术方案中,所述导电基底卷呈圆筒状。In the above technical solution, the conductive substrate roll is cylindrical.

本实用新型的有益效果是:The beneficial effects of the utility model are:

本实用新型提供了一种应用于有机物氧化中的阳极催化剂的制备装置,可用于制备电解水阳极氧化有机物和电催化析氧反应耦合阴极制氢的催化剂,制备装置结构简单,可以实现温和条件下快速制备大面积催化剂,且装置清洁环保,利用装置合成的催化剂性能优异。The utility model provides a preparation device for an anode catalyst used in the oxidation of organic matter, which can be used to prepare catalysts for the anode oxidation of organic matter by electrolysis of water and the coupled cathode hydrogen production by electrocatalytic oxygen evolution reaction. The preparation device has a simple structure and can realize the rapid preparation of large-area catalysts under mild conditions. The device is clean and environmentally friendly, and the catalyst synthesized by the device has excellent performance.

附图说明BRIEF DESCRIPTION OF THE DRAWINGS

图1是本实用新型的结构示意图;Fig. 1 is a schematic diagram of the structure of the utility model;

图2是应用实例1得到的Ni(OH)2催化剂的实物照片;FIG2 is a physical photograph of the Ni(OH) 2 catalyst obtained in Application Example 1;

图3是应用实例1得到的Ni(OH)2催化剂的扫描电子显微镜照片;FIG3 is a scanning electron microscope photograph of the Ni(OH) 2 catalyst obtained in Application Example 1;

图4是应用实例1得到的Ni(OH)2催化剂与经过清洗后的泡沫镍催化析氧反应性能对比图。FIG. 4 is a comparison chart of the oxygen evolution reaction performance of the Ni(OH) 2 catalyst obtained in Application Example 1 and the cleaned nickel foam.

其中:in:

1 加热装置 2 反应器1 Heating device 2 Reactor

3 层析柱 4 泵3 Chromatography column 4 Pump

5 质子交换膜电解槽 6 直流电源5 Proton exchange membrane electrolyzer 6 DC power supply

7 输出管 8 输入管7 Output pipe 8 Input pipe

9隔板 10导电基底。9 separator 10 conductive substrate.

对于本领域普通技术人员来讲,在不付出创造性劳动的前提下,可以根据以上附图获得其他的相关附图。For ordinary technicians in this field, other relevant drawings can be obtained based on the above drawings without any creative work.

具体实施方式DETAILED DESCRIPTION

为了使本技术领域的人员更好地理解本实用新型技术方案,下面结合说明书附图并通过具体实施方式来进一步说明本实用新型的技术方案。In order to enable those skilled in the art to better understand the technical solution of the present invention, the technical solution of the present invention is further described below in conjunction with the accompanying drawings and through specific implementation methods.

如图1所示,一种应用于有机物氧化中的阳极催化剂的制备装置,包括反应机构和电解机构,所述反应机构包括加热装置1、放置于加热装置1的加热腔内的反应器2以及置于反应器2上方的层析柱3;所述电解机构包括质子交换膜电解槽5以及为其供能的直流电源6;质子交换膜电解槽5的进料口与反应器2出口通过输出管7连接,质子交换膜电解槽5的出料口与层析柱3进气口通过输入管8连接;导电基底10放置于层析柱3内,且位于隔板9上方。As shown in Figure 1, a preparation device for an anode catalyst used in the oxidation of organic matter includes a reaction mechanism and an electrolysis mechanism, wherein the reaction mechanism includes a heating device 1, a reactor 2 placed in a heating chamber of the heating device 1, and a chromatography column 3 placed above the reactor 2; the electrolysis mechanism includes a proton exchange membrane electrolyzer 5 and a DC power supply 6 for powering it; the feed inlet of the proton exchange membrane electrolyzer 5 is connected to the outlet of the reactor 2 through an output pipe 7, and the discharge port of the proton exchange membrane electrolyzer 5 is connected to the air inlet of the chromatography column 3 through an input pipe 8; a conductive substrate 10 is placed in the chromatography column 3 and is located above the partition 9.

所述输出管7上设置泵4,输出管7一端伸入反应器2内部,且位于液面上方,输出管7与反应器2的出口之间通过密封件密封。The pump 4 is arranged on the output pipe 7 , one end of the output pipe 7 extends into the reactor 2 and is located above the liquid surface, and the output pipe 7 and the outlet of the reactor 2 are sealed by a sealing member.

所述层析柱3顶端敞口,且设置可拆卸密封盖。The top of the chromatography column 3 is open and is provided with a detachable sealing cover.

所述层析柱3进气口设置于隔板9下方。The gas inlet of the chromatography column 3 is arranged below the partition 9 .

所述层析柱3下端插入反应器2内,且两者之间密封处理。The lower end of the chromatography column 3 is inserted into the reactor 2, and the two are sealed.

所述直流电源6正极通过电线连接质子交换膜电解槽5的阳极板,其负极通过电线连接质子交换膜电解槽5的阴极板。The positive electrode of the DC power supply 6 is connected to the anode plate of the proton exchange membrane electrolyzer 5 through an electric wire, and the negative electrode thereof is connected to the cathode plate of the proton exchange membrane electrolyzer 5 through an electric wire.

所述质子交换膜电解槽5的进料口和出料口均设置于阳极板侧。The feed inlet and the discharge outlet of the proton exchange membrane electrolyzer 5 are both arranged on the anode plate side.

所述导电基底10卷呈圆筒状。The conductive substrate 10 is rolled into a cylindrical shape.

在本实施例中,所述反应器为两口圆底烧瓶,所述加热装置为加热台。In this embodiment, the reactor is a two-necked round-bottom flask, and the heating device is a heating table.

应用实例1Application Example 1

(1)对8000cm2泡沫镍使用乙醇清洗液浸泡,超声处理20min,取出后用去离子水冲洗干净,再放入0.2mol/L的硫酸溶液中浸泡20min,清洗完取出使用去离子水清洗至表面无硫酸残留,处理后的导电基底10(泡沫镍)卷呈圆筒状后放入层析柱3内,盖上层析柱密封盖;(1) 8000 cm 2 of nickel foam was soaked in an ethanol cleaning solution, ultrasonically treated for 20 min, taken out and rinsed with deionized water, and then soaked in a 0.2 mol/L sulfuric acid solution for 20 min. After washing, it was taken out and washed with deionized water until no sulfuric acid residue was left on the surface. The treated conductive substrate 10 (nickel foam) was rolled into a cylindrical shape and placed in a chromatography column 3, and the chromatography column sealing cover was covered;

(2)将去离子水放入反应器2(圆底烧瓶)内,组装装置其余器件;(2) Place deionized water into reactor 2 (round-bottom flask) and assemble the remaining components of the device;

(3)开启加热装置1对反应器2内的去离子水加热至80℃,加热后的去离子水通过泵4以5mL*min-1的流速通入质子交换膜电解槽5中,对质子交换膜电解槽5施加6A电流,质子交换膜电解槽5产生的氧气和电解槽出口流出的去离子水通入层析柱3进气口,去离子水流回反应器2(圆底烧瓶)内,氧气和水蒸气的混合气充满反应器2和层析柱3内,处理后的导电基底在氧气和水蒸气混合气中腐蚀4h,取出后在60℃烘箱中干燥1h后即得应用于有机物氧化中的阳极催化剂。(3) Turn on the heating device 1 to heat the deionized water in the reactor 2 to 80° C. The heated deionized water is passed into the proton exchange membrane electrolyzer 5 at a flow rate of 5 mL*min -1 through the pump 4. A current of 6 A is applied to the proton exchange membrane electrolyzer 5. The oxygen generated by the proton exchange membrane electrolyzer 5 and the deionized water flowing out of the electrolyzer outlet are passed into the air inlet of the chromatography column 3. The deionized water flows back into the reactor 2 (round-bottom flask). The mixed gas of oxygen and water vapor fills the reactor 2 and the chromatography column 3. The treated conductive substrate is corroded in the mixed gas of oxygen and water vapor for 4 h. After being taken out, it is dried in an oven at 60° C. for 1 h to obtain an anode catalyst used in the oxidation of organic matter.

所制备的阳极催化剂的实物照片如图2所示,Ni(OH)2催化剂的扫描电子显微镜照片如图3所示,应用实例1得到的Ni(OH)2催化剂与经过清洗后的泡沫镍催化析氧反应性能对比如图4所示,可见本实用新型装置可以快速制备大面积催化剂,且制备催化剂均匀,性能优异。A physical photograph of the prepared anode catalyst is shown in FIG2 , a scanning electron microscope photograph of the Ni(OH) 2 catalyst is shown in FIG3 , and a comparison of the oxygen evolution reaction performance of the Ni(OH) 2 catalyst obtained in Application Example 1 and the cleaned nickel foam is shown in FIG4 . It can be seen that the utility model device can quickly prepare large-area catalysts, and the prepared catalysts are uniform and have excellent performance.

需要说明的是,在不冲突的情况下,本实用新型中的实施例及实施例中的特征可以相互组合。It should be noted that, in the absence of conflict, the embodiments of the present invention and the features in the embodiments can be combined with each other.

在本实用新型的描述中,需要理解的是,术语“中心”、“纵向”、“横向”、“上”、“下”、“前”、“后”、“左”、“右”、“竖直”、“水平”、“顶”、“底”、“内”、“外”等指示的方位或位置关系为基于附图所示的方位或位置关系,仅是为了便于描述本实用新型和简化描述,而不是指示或暗示所指的装置或元件必须具有特定的方位、以特定的方位构造和操作,因此不能理解为对本实用新型的限制。此外,术语“第一”、“第二”等仅用于描述目的,而不能理解为指示或暗示相对重要性或者隐含指明所指示的技术特征的数量。由此,限定有“第一”、“第二”等的特征可以明示或者隐含地包括一个或者更多个该特征。在本实用新型的描述中,除非另有说明,“多个”的含义是两个或两个以上。In the description of the present utility model, it should be understood that the terms "center", "longitudinal", "lateral", "up", "down", "front", "back", "left", "right", "vertical", "horizontal", "top", "bottom", "inside", "outside" and the like indicate positions or positional relationships based on the positions or positional relationships shown in the accompanying drawings, and are only for the convenience of describing the present utility model and simplifying the description, rather than indicating or implying that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and therefore cannot be understood as a limitation on the present utility model. In addition, the terms "first", "second", etc. are only used for descriptive purposes, and cannot be understood as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Therefore, features defined as "first", "second", etc. may explicitly or implicitly include one or more of the features. In the description of the present utility model, unless otherwise specified, "multiple" means two or more.

在本实用新型的描述中,需要说明的是,除非另有明确的规定和限定,术语“安装”、“相连”、“连接”应做广义理解,例如,可以是固定连接,也可以是可拆卸连接,或一体地连接;可以是机械连接,也可以是电连接;可以是直接相连,也可以通过中间媒介间接相连,可以是两个元件内部的连通。对于本领域的普通技术人员而言,可以通过具体情况理解上述术语在本实用新型中的具体含义。In the description of the present invention, it should be noted that, unless otherwise clearly specified and limited, the terms "installation", "connection" and "connection" should be understood in a broad sense, for example, it can be a fixed connection, a detachable connection, or an integral connection; it can be a mechanical connection or an electrical connection; it can be a direct connection, or it can be an indirect connection through an intermediate medium, or it can be the internal communication of two components. For ordinary technicians in this field, the specific meanings of the above terms in the present invention can be understood by specific circumstances.

申请人声明,以上所述仅为本实用新型的具体实施方式,但本实用新型的保护范围并不局限于此,所属技术领域的技术人员应该明了,任何属于本技术领域的技术人员在本实用新型揭露的技术范围内,可轻易想到的变化或替换,均落在本实用新型的保护范围和公开范围之内。The applicant declares that the above is only a specific implementation method of the present utility model, but the protection scope of the present utility model is not limited thereto. Technical personnel in the relevant technical field should understand that any changes or substitutions that can be easily thought of by technical personnel in the relevant technical field within the technical scope disclosed in the present utility model fall within the protection scope and disclosure scope of the present utility model.

Claims (6)

1. The preparation device of the anode catalyst applied to the oxidation of the organic matters is characterized in that: the device comprises a reaction mechanism and an electrolysis mechanism, wherein the reaction mechanism comprises a heating device (1), a reactor (2) arranged in a heating cavity of the heating device (1) and a chromatographic column (3) arranged above the reactor (2); the electrolysis mechanism comprises a proton exchange membrane electrolysis cell (5) and a direct current power supply (6) for supplying power to the proton exchange membrane electrolysis cell; the feed inlet of the proton exchange membrane electrolytic cell (5) is connected with the outlet of the reactor (2) through an output pipe (7), and the discharge outlet of the proton exchange membrane electrolytic cell (5) is connected with the air inlet of the chromatographic column (3) through an input pipe (8); the conductive substrate (10) is placed in the chromatographic column (3).
2. The preparation device of the anode catalyst applied to the oxidation of organic matters according to claim 1, wherein: the conductive substrate (10) is placed above the partition plate (9) of the chromatographic column (3), and the conductive substrate (10) is rolled into a cylinder shape.
3. The preparation device of the anode catalyst applied to the oxidation of organic matters according to claim 1, wherein: the output pipe (7) is provided with a pump (4), one end of the output pipe (7) extends into the reactor (2) and is positioned above the liquid level, and the output pipe (7) is sealed with the outlet of the reactor (2) through a sealing piece.
4. The preparation device of the anode catalyst applied to the oxidation of organic matters according to claim 1, wherein: the top end of the chromatographic column (3) is open, and a detachable sealing cover is arranged; the air inlet of the chromatographic column (3) is arranged below the partition board (9), the lower end of the chromatographic column (3) is inserted into the reactor (2), and the two are sealed.
5. The preparation device of the anode catalyst applied to the oxidation of organic matters according to claim 1, wherein: the positive electrode of the direct current power supply (6) is connected with the positive plate of the proton exchange membrane electrolytic tank (5) through an electric wire, and the negative electrode of the direct current power supply is connected with the negative plate of the proton exchange membrane electrolytic tank (5) through an electric wire.
6. The preparation device of the anode catalyst applied to the oxidation of organic matters according to claim 1, wherein: the feed inlet and the discharge outlet of the proton exchange membrane electrolytic tank (5) are arranged at the anode plate side.
CN202323528686.5U 2023-12-25 2023-12-25 A device for preparing anode catalyst used in organic matter oxidation Active CN221663030U (en)

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