WO2021062940A1

WO2021062940A1 - Continuous dispersion system, catalyst batch synthesis apparatus and method

Info

Publication number: WO2021062940A1
Application number: PCT/CN2019/123880
Authority: WO
Inventors: 王中奇; 高正飞
Original assignee: 青岛创启新能催化科技有限公司
Priority date: 2019-09-30
Filing date: 2019-12-09
Publication date: 2021-04-08
Also published as: CN110639415A

Abstract

The present invention relates to a continuous dispersion system, a carbon carrier dispersion apparatus, and a catalyst synthesis apparatus and method. The continuous dispersion system comprises a stirring module, an ultrasonic module, and a material circulation mechanism. The power of the ultrasonic module is not less than 500 W, and is used for dispersing materials. The stirring module is used for dispersing materials. The material circulation mechanism communicates the ultrasonic module with the stirring module, so that the materials in the ultrasonic module and the stirring module can circulate with each other. According to the continuous dispersion system, on the one hand, the ultrasonic module and the stirring module together disperse the materials to maintain the uniform dispersion of the materials in the continuous dispersion system; on the other hand, the heat conduction of nanoscale ultrafine dispersion is accelerated by circulating the stirring module and the ultrasonic module. This is circularly repeated, so that the mass dispersion of the materials is proceeded smoothly, and the dispersion effect of the mass dispersion is greatly improved, thereby improving the production efficiency of nanomaterial synthesis.

Description

Continuous dispersion system, catalyst batch synthesis device and method

Technical field

The invention relates to the technical field of nanomaterials, in particular to a continuous dispersion system, a carbon carrier dispersion device, a catalyst synthesis device and a method.

Background technique

In the field of liquid-phase synthesis of nanomaterials, in order to avoid agglomeration of nanomaterials, the control of dispersion uniformity has always been the core step of the synthesis, because it directly determines the properties of the material.

In the field of catalyst synthesis, the control of the dispersion uniformity of nanomaterials is more prominent. The improvement of the catalytic performance of the catalyst is largely limited by the dispersibility of the material. In the early stage of the development of catalyst materials, the amount of synthesis in the laboratory is generally tens of milligrams, and the amount of support material required is relatively small and the dispersion is relatively easy. However, in the mass production stage, the difficulty of controlling the uniformity of dispersion increases sharply. The decentralized control effect of the original laboratory is weakened, and the improvement of the control conditions greatly increases the requirements for the experimental environment and experimental equipment. At the same time, the risk of the experiment is greatly increased, and the development difficulty of the mass production process is significantly increased. The existing technology needs to be further improved and optimized in the mass production of nanomaterials.

Summary of the invention

Based on this, the present invention provides a continuous dispersion system, a carbon carrier dispersion device, a catalyst synthesis device and a method that can improve the dispersion effect of mass dispersion.

A continuous decentralized system, including:

Ultrasonic module, the power of the ultrasonic module is not less than 500W, used to disperse materials;

Stirring module, used to disperse materials;

The material circulation mechanism connects the ultrasonic module with the stirring module, so that the materials in the ultrasonic module and the stirring module can circulate and circulate with each other.

On the one hand, the above-mentioned continuous dispersion system uses the ultrasonic module and the stirring module to disperse the materials to maintain the uniform dispersion of the materials in the continuous dispersion system. It enters the ultrasonic module for further ultra-fine dispersion, and the material that passes through the ultrasonic module for further ultra-fine dispersion can also enter the stirring module for further refinement and uniformity. At the same time, it also accelerates the conduction of ultra-fine dispersion heat, so that the material is reciprocated. The large-scale dispersion of nano-materials can be carried out smoothly, and the dispersion effect of the large-scale dispersion is greatly improved, and the production efficiency of nano-material synthesis can be improved.

In some of the embodiments, the ultrasonic module includes a material containing mechanism communicating with the material circulating mechanism and at least a part of an ultrasonic mechanism provided inside the material containing mechanism.

In some of the embodiments, the continuous dispersion system further includes a heat dissipation mechanism for cooling and dissipating the ultrasonic module.

In some of the embodiments, the heat dissipation mechanism includes a cooling medium circulation pipeline and a cooling medium circulation pump arranged on the cooling medium circulation pipeline.

In some of the embodiments, the heat dissipation mechanism further includes a cooling medium containing mechanism arranged outside the material containing mechanism, so that the outside of the material containing mechanism can be immersed in the cooling medium of the cooling medium containing mechanism, The cooling medium accommodating mechanism is connected in series with the cooling medium circulation pipeline.

In some of the embodiments, the cooling medium containment mechanism and the material containment mechanism are an integrated structure, and the material containment mechanism is a shell with a containment cavity, and the containment cavity is used to contain the material for ultrasound. The housing includes an outer wall and an inner wall, and an interlayer space for accommodating a cooling medium is formed between the outer wall and the inner wall.

In some of the embodiments, the inner wall is further provided with a material circulation inlet and a material circulation outlet communicating with the accommodating cavity and the material circulation mechanism, and at least part of the material circulation mechanism is located in the interlayer space .

In some of the embodiments, the continuous dispersion system includes at least two of the ultrasonic modules, and each of the ultrasonic modules is connected in series.

In some of the embodiments, the material circulation mechanism includes a material circulation pump and a material circulation pipeline, the material circulation pipeline is connected between the ultrasonic module and the stirring module, and the material circulation pump is installed in the The material circulation pipeline.

In some of the embodiments, the material circulation mechanism further includes a first control valve and a second control valve. The first control valve is provided between one end of the ultrasonic module and the material between the stirring module connected to it. On the circulation pipeline, the second control valve is arranged on the material circulation pipeline between the other end of the ultrasonic module and the stirring module connected with it.

In some of the embodiments, the power of the ultrasound module is not less than 1000W.

A carbon carrier dispersion device includes an initial dispersion mechanism and any one of the above-mentioned continuous dispersion systems. The material circulation mechanism is provided with an inlet, and the initial dispersion mechanism is in communication with the inlet.

In some of the embodiments, the preliminary dispersion mechanism is a high-speed shearing device.

A catalyst synthesis device, comprising the above-mentioned carbon carrier dispersion device, a reaction kettle and a catalyst collection device connected in sequence with the carbon carrier dispersion device, a discharge port is provided on the material circulation mechanism, and the output of the material circulation mechanism The feed port is in communication with the reaction kettle.

A method for batch synthesis of a catalyst, which uses the above-mentioned catalyst synthesis device to synthesize a catalyst in batch, including:

Cleaning and drying the catalyst synthesis device, adding a predetermined amount of solvent and carbon black to the preliminary dispersion mechanism, and turning on the stirring;

Stir for a predetermined time to form a suspension. When there is no obvious solid deposit at the bottom of the initial dispersion mechanism, open the feed inlet to allow the suspension to enter and fill the continuous dispersion system, close the feed inlet, and turn on the ultrasonic module, The stirring module and the material circulation mechanism make the material continuously circulate ultrasonically for a predetermined time in the continuous dispersion system to form a uniformly dispersed carbon carrier dispersion;

Open the discharge port, make the carbon carrier dispersion enter the reactor, add or pre-add the catalyst precursor material and the solvent at the same time, continue to stir, control the temperature, and start the catalyst synthesis reaction;

After the reaction is completed, the mixture in the reactor is introduced into the catalyst collection device and filtered to obtain the primary catalyst; and

The primary catalyst is subjected to post-treatment to obtain a catalyst product.

The catalyst synthesis process provided by the invention can be mass-produced continuously, and the obtained catalyst product has high dispersion uniformity.

Description of the drawings

Figure 1 is a schematic structural diagram of a continuous dispersion system according to an embodiment;

Figure 2 is a schematic structural diagram of a catalyst synthesis device in an embodiment;

Figure 3 is a scanning electron micrograph of the catalyst product prepared in Example 1;

Figure 4 is a scanning electron micrograph of the catalyst product prepared in Comparative Example 1;

Figure 5 is a scanning electron micrograph of the catalyst product prepared in Comparative Example 2.

Detailed ways

In order to facilitate the understanding of the present invention, the present invention will be more fully described below with reference to the relevant drawings. The preferred embodiments of the present invention are shown in the drawings. However, the present invention can be implemented in many different forms and is not limited to the embodiments described herein. On the contrary, the purpose of providing these embodiments is to make the understanding of the disclosure of the present invention more thorough and comprehensive.

It should be noted that when an element is referred to as being "fixed to" another element, it can be directly on the other element or a central element may also be present. When an element is considered to be "connected" to another element, it can be directly connected to the other element or an intermediate element may be present at the same time.

Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by those skilled in the technical field of the present invention. The terms used in the description of the present invention herein are only for the purpose of describing specific embodiments, and are not intended to limit the present invention. The term "and/or" as used herein includes any and all combinations of one or more related listed items.

Technicians have found that the use of high-speed shear emulsification and dispersion of large quantities of carrier materials alone cannot disperse agglomerated nano-scale materials to nano-scale. However, if the ultrasonic device is used alone, only a small batch of agglomerated nano-scale materials can be dispersed to the nano-scale; if a large-scale dispersion is performed, a large amount of heat will be generated. Highly active carrier materials (such as carbon carrier materials) are extremely inefficient after generating a large amount of heat. Safe and easy to explode. In addition, the power of the ultrasonic device used for nano-scale crushing is relatively large, which will also bring noise and heat, and further increase the difficulty of mass dispersion. There is still a problem of ultrasonic efficiency in large-scale high-power ultrasonic dispersion. How to effectively use ultrasonic energy and improve ultrasonic efficiency is an urgent problem to be solved.

Please refer to FIG. 1, an embodiment of the present invention provides an embodiment of a continuous dispersion system 100, which includes a stirring module 110, an ultrasonic module 120, and a material circulation mechanism (not shown in the figure).

Among them, the stirring module 110 is used to disperse materials, so that the materials maintain the uniformity of dispersion in the flow, and avoid agglomeration and loss of ultrasonic effect. The power of the ultrasonic module 120 is 1200W, which is used to implement high-power ultrasonic dispersion of materials.

The material circulation mechanism connects the stirring module 110 and the ultrasonic module 120 so that the materials in the stirring module 110 and the ultrasonic module 120 can circulate with each other to form a flowing dispersion system. The fluid dispersion system proposed in the present invention helps to circulate multiple times of ultrasound and improves the efficiency of ultrasound; at the same time, it helps to take out the heat caused by the ultrasound and reduce the accumulation of heat in the ultrasound module, thereby causing danger.

On the one hand, the continuous dispersion system 100 uses the ultrasonic module 120 and the stirring module 110 to disperse the materials to maintain the uniform dispersion of the materials in the continuous dispersion system 100, and on the other hand, the stirring module 110 and the ultrasonic module 120 are circulated through the material circulation mechanism, so that the stirring module 110 The uniformly refined material can enter the ultrasonic module 120 for further ultra-fine dispersion, and the material that has been further ultra-finely dispersed through the ultrasonic module 120 can also enter the stirring module 110 for further refinement, and at the same time accelerates the ultra-fine dispersion. The conduction of heat, cyclically and repeatedly, enables the mass dispersion of materials to proceed smoothly, and greatly improves the dispersion effect of mass dispersion, thereby improving the production efficiency of nanomaterial synthesis.

The present invention focuses on the overall design of the continuous dispersion system, and fully considers the formation of dispersion uniformity, dispersion uniformity control, heat dispersion, continuous production and other factors, and proposes an overall design plan.

In particular, the continuous dispersion system 100 described above can be used to disperse large quantities of nano-scale carrier materials, such as nano-scale carbon materials.

In some examples, the stirring module 110 is a magnetic stirring module or a mechanical stirring module. In a specific example, the stirring module 110 is a magnetic stirrer.

In other examples, the stirring module 110 is an ultrasonic stirrer with a power of about 200W.

In some examples, the power of the ultrasound module 120 is not less than 1000W.

In some embodiments, the ultrasonic module 120 includes a material containing mechanism 121 communicating with the material circulating mechanism and an ultrasonic mechanism 122 at least partially disposed inside the material containing mechanism. The ultrasonic mechanism 122 is used to generate ultrasonic waves to perform high-power ultrasonic dispersion of the material in the material containing mechanism 121. The material containing mechanism 121 provides a place for material dispersion, and the ultrasonic mechanism 122 provides ultrasonic waves for material dispersion.

In some embodiments, the number of ultrasonic modules 120 is multiple (more than two), the multiple ultrasonic modules 120 are connected in series, and each ultrasonic module 120 and the stirring module 110 are connected through a material circulation mechanism. In this way, a multi-level dispersion system is formed by a plurality of ultrasonic modules 120, which can further improve the nano-level dispersion effect. In addition, the multi-stage ultrasonic dispersion system can also reduce the ultrasonic power of the ultrasonic module 120.

For example, in a specific example, the ultrasonic module 120 is an ultrasonic device or an ultrasonic disperser.

It can be understood that, in addition to the material containing mechanism 121 and the ultrasonic mechanism 122, the ultrasonic device also has an ultrasonic horn. The ultrasonic horn is preferably a low-power ultrasonic horn. By setting up a multi-stage ultrasonic device, it can carry out 100g batches of carbon. Material handling.

Further, the number of ultrasound modules 120 is multiple, and the multiple ultrasound modules 120 are arranged adjacent to each other in sequence.

In some of the embodiments, the continuous dispersion system 100 further includes a heat dissipation mechanism, which is used to cool the ultrasonic module 120 and dissipate heat, which can further reduce the risk of explosion caused by the accumulation of nano-scale ultra-fine dispersion heat of the material.

Further, the heat dissipation mechanism includes a cooling medium circulating pump (not shown) and a cooling medium circulating pipe 141. The cooling medium circulating pipe 141 is used to cool the ultrasonic module 120, and the cooling medium circulating pump is installed on the cooling medium circulating pipe 141.

Among them, the cooling medium circulation pipeline 141 is used to store and circulate the cooling medium, such as cooling water.

When the number of ultrasonic modules 120 is multiple, the heat dissipation mechanism can simultaneously heat the multiple ultrasonic modules 120.

Further, the heat dissipation mechanism further includes a cooling medium containing mechanism 142 arranged outside the material containing mechanism 121, so that the outside of the material containing mechanism 121 can be immersed in the cooling medium of the cooling medium containing mechanism 142. The cooling medium containing mechanism 142 and the cooling medium The circulation pipeline 141 is connected in series to circulate the cooling medium, which can further improve the heat dissipation effect.

In a specific embodiment, as shown in FIG. 1, the ultrasonic module 120 includes three ultrasonic dispersers connected in series, and the power of each ultrasonic disperser is 500-800W. The outer surfaces of the three ultrasonic dispersers are also provided with a heat dissipation mechanism. .

In a preferred embodiment, in a continuous dispersion system, the ultrasonic module 120 and the stirring module 110 are arranged at intervals, for example, the number of the ultrasonic module 120 and the stirring module 110 is three. The material flows through the first ultrasonic module 120, the first stirring module 110, the second ultrasonic module 120, the second stirring module 110, the third ultrasonic module 120, and the third stirring module 110 in turn, each ultrasonic module 120 The power is not less than 800W, and then flows into the reactor of the catalyst synthesis device through the discharge port.

Further, the heat dissipation mechanism and the ultrasonic disperser are an integrated device. The material containing mechanism 121 in the ultrasonic disperser is a shell with a containing cavity. The accommodating cavity is used for accommodating materials for ultrasound. The housing includes an outer wall and an inner wall, and an interlayer space for accommodating a cooling medium is formed between the outer wall and the inner wall. The housing with the interlayer space is therefore also equivalent to the cooling medium accommodating mechanism 142 of the heat dissipation mechanism. In other words, the cooling medium accommodating mechanism 142 of the heat dissipation mechanism and the material accommodating mechanism 121 of the ultrasonic module are an integrated structure.

Specifically, the outer wall is also provided with a cooling medium inlet and a cooling medium outlet, so that the cooling medium communicates in the interlayer space.

Specifically, the inner wall is also provided with a material circulation inlet and a material circulation outlet communicating with the accommodating cavity and the material circulation mechanism, so that the material is circulated and communicated among the material containing mechanism 121, the material circulation mechanism and the stirring module 110.

Specifically, at least part of the material circulation mechanism is located in the interlayer space. In this way, the cooling medium in the interlayer space can not only cool and dissipate the materials in the accommodating cavity, but also cool and dissipate the materials in the material circulation mechanism at the same time.

Specifically, the material circulation pipeline 131 (see below) of the material circulation mechanism passes through the interlayer space formed by the outer wall and the inner wall of the housing and communicates with the material circulation inlet and the material circulation outlet on the inner wall respectively, so that the material circulation pipeline 131 The material in the accommodating cavity is connected with the material in the accommodating cavity. In this way, the cooling medium in the interlayer space can not only cool and dissipate the materials in the accommodating cavity, but also cool and dissipate the materials in the material circulation pipeline 13 at the same time. In some embodiments, the material circulation mechanism includes a material circulation pump (not shown) and a material circulation pipe 131. The material circulation pipe 131 is connected between the ultrasonic module 120 and the stirring module 110, and the material circulation pump is installed in the material circulation pipe. On the road 131. In this way, the material circulation between the ultrasonic module 120 and the stirring module 110 is realized through the material circulation pump and the material circulation pipeline 131.

Furthermore, the material circulation mechanism further includes a first control valve 132 and a second control valve 133. The first control valve 132 is provided on the material circulation pipeline 131 between one end of the ultrasonic module 120 and the stirring module 110 connected to it. The second control valve 133 is provided on the material circulation pipeline 131 between the other end of the ultrasonic module 120 and the stirring module 110 connected to it. In this way, the flow of materials is controlled by two control valves.

One end and the other end of the mixing module 110 are the two ends of the mixing module 110 and the material circulation pipeline 131. Specifically, one end is used for the material to enter the mixing module 110 from the material circulation pipeline 131, and the other end is used for the material to enter the material circulation pipeline 131 from the mixing module 110.

Further, in the continuous dispersion system 100, the material inlet can be set in the stirring module 110 or the ultrasonic module 120. The material is first added in the stirring module 110 or the ultrasonic module 120, and then circulated among the dispersion mechanisms through the material circulation mechanism. Specifically, in this example, the material inlet is set on the mixing module 110.

An embodiment of the present invention also provides an embodiment of a carbon carrier dispersion device, which includes an initial dispersion mechanism and any of the above-mentioned continuous dispersion systems. Among them, the material circulation mechanism in the continuous dispersion system is provided with an inlet, and the initial dispersion mechanism is connected with the inlet.

In a specific example, the primary dispersion mechanism is a high-speed shearing device, such as a high-speed shearing emulsifier. It can be understood that the primary dispersion mechanism is not limited to this, and may also be other homogenizers.

1 and FIG. 2, an embodiment of the present invention also provides an example of a catalyst synthesis device 10, which includes any one of the continuous dispersion system 100, a reactor 200, and a catalyst collection device 300 connected in sequence. The material circulation mechanism is provided with a discharge port 1301, and the discharge port of the material circulation mechanism is in communication with the reactor 200.

Furthermore, the discharge port 1301 of the material circulation pipeline 131 is used for discharging the dispersed materials of the continuous dispersion system 100. Furthermore, in order to control the opening and closing of the discharge port 1301, a third control valve (not shown in the figure) may be provided at the discharge port.

The reactor 200 is used for material reaction to obtain a catalyst, and the catalyst collecting device 300 is used for collecting the catalyst.

Specifically, the continuous dispersion system 100 is in communication with the reactor 200 through a discharge port 1301.

Further, the catalyst collecting device 300 is a filtering device, and the catalyst collecting device 300 is provided at the outlet end of the discharging pipeline of the reactor 200.

Specifically, the catalyst collection device 300 includes a collection funnel (not shown in the figure) and a filter screen (not shown in the figure). The collection funnel is installed at the outlet end of the feeding pipe of the reactor 200, and the filter screen is installed on the collection funnel. The liquid phase is filtered, and the solid phase, the catalyst, is collected. The catalyst synthesis device 10 further includes a first waste collection device 400 for collecting the liquid-phase waste liquid filtered by the catalyst collection device 300.

Further, the catalyst synthesis device 10 further includes a second waste collection device 500 which is connected to the reactor 200 for collecting waste liquid in the reactor 200.

The above-mentioned continuous dispersion system 100 can be used for the dispersion of support materials in catalyst synthesis, such as nano-scale carbon support materials. The above-mentioned catalyst synthesis device 10 can be used for catalyst synthesis. A single batch can synthesize more than 200g of catalyst, and it can synthesize more than 400g of catalyst per day.

Correspondingly, a method for dispersing materials by using the above continuous dispersion system 100 or a method for synthesizing a catalyst using the above catalyst synthesis device 10 is provided.

An embodiment of the present invention also provides an example of a catalyst batch synthesis method. The catalyst synthesis device is used to synthesize a catalyst in batch. The catalyst batch synthesis method includes the following steps:

Step 1: Clean and dry the catalyst synthesis device, add a predetermined amount of solvent and carbon black to the preliminary dispersion mechanism, and start stirring.

Step 2: Stir for a predetermined time to form a suspension. When there is no obvious solid deposit at the bottom of the initial dispersion mechanism, open the feed inlet to allow the suspension to enter and fill the continuous dispersion system, close the feed inlet, turn on the ultrasonic module, and stir The module and the material circulation mechanism make the materials circulate in the continuous dispersion system for a predetermined time and form a uniformly dispersed carbon carrier dispersion.

Step 3: Open the discharge port, make the carbon carrier dispersion enter the reactor, add or pre-add the catalyst precursor material and the solvent at the same time, continue to stir, control the temperature, and start the catalyst synthesis reaction.

Step 4: After the reaction is completed, the mixture in the reactor is introduced into the catalyst collecting device, and filtered to obtain the primary catalyst.

Step 5: Post-processing the primary catalyst to obtain a catalyst product.

In a specific embodiment, the catalyst precursor material, the reducing agent, and the carbon dispersion carrier passing through the continuous dispersion system are respectively flowed to the catalyst reaction vessel, and the flow rate of the carbon dispersion carrier, the catalyst precursor material and the reducing agent flowing into the reaction vessel is controlled. The proportion of reaction materials.

In order to better illustrate the beneficial effects of the continuous dispersion system, the following is a specific embodiment of using the continuous dispersion system 100 for material dispersion.

Specific Example 1

The catalyst synthesis device shown in FIG. 2 is used, which includes a continuous dispersion system 100, a reactor 200, a catalyst collection device 300, a first waste collection device 400, a second waste collection device 500, and a preliminary dispersion device (not shown in the figure) ). The continuous dispersion system 100 is shown in FIG. 1. Among them, the stirring module 110 is a magnetic stirrer, and the ultrasonic module 120 is a 1200W ultrasonic instrument. The initial dispersing device is a shearing emulsifying device, which is connected to the inlet of the continuous dispersing system and controlled by a valve.

Step 1: Clean and dry the catalyst synthesis device. The first control valve 132 and the second control valve 133 are closed. Add 5L of solvent (H2O) to the high-speed shearing emulsifier, weigh 10g of carbon black (EC300J, Lion), put it into the high-speed shearing emulsifier, and turn on the stirring .

Step 2: Stir the material in the high-speed shearing emulsifier for 30 minutes to form a suspension. When there is no obvious solid deposit at the bottom of the high-speed shearing emulsifier, open the inlet of the continuous dispersion system to make the material enter the continuous dispersion system. The first control valve 132 and the second control valve 133 are opened to allow the suspension to circulate to the ultrasonic modules 120 through the material circulation mechanism. After the material flow is stable, the ultrasonic device is started. After 30 minutes of sonication, it was confirmed that the liquid in the ultrasonic device had no obvious suspended particles. If there are suspended particles, open the first control valve 132 and the second control valve 133 and continue to enter the high-speed shear emulsifier to start stirring, and so on, until the liquid in the ultrasonic device has no obvious suspended particles.

Step 3: Open the third control valve to open the discharge port, and introduce all the suspension into the ultrasonic device between the continuous dispersion system and the reaction kettle for further dispersion.

Step 4: Then, after introducing the suspension into the reaction kettle, continue to stir, control the temperature, and add a predetermined quantity of platinum salt and a reducing agent to react. After reacting for 1 hour, the mixture in the reaction kettle is introduced into the catalyst collection device and filtered to obtain the primary catalyst.

Step 5: Post-processing the primary catalyst to obtain a catalyst product.

Comparative example 1

Comparative Example 1 Use high-speed shear emulsification alone to disperse 10g carbon black in 5L solvent (H ₂ O), add the resulting suspension to a single 200W ultrasonic disperser for dispersion for 1 hour, and then transfer the ultrasonic dispersion Into the reactor, continue to stir, control the temperature, and add a predetermined mass of platinum salt and a reducing agent to react. After reacting for 1 hour, the mixture in the reaction kettle is introduced into the catalyst collection device and filtered to obtain the primary catalyst. The primary catalyst is subjected to post-treatment to obtain a catalyst product.

Comparative example 2

Comparative Example 2 Use high-speed shear emulsification alone to disperse 10g carbon black in 5L solvent (H ₂ O), and then transfer the ultrasonic dispersion to the reactor, continue to stir, control the temperature, and add a predetermined quality of platinum salt and The reducing agent reacts. After reacting for 1 hour, the mixture in the reaction kettle is introduced into the catalyst collection device and filtered to obtain the primary catalyst. The primary catalyst is subjected to post-treatment to obtain a catalyst product.

The catalyst products prepared in Example 1 and Comparative Example 1 and Comparative Example 2 were characterized by scanning transmission electron microscopy, and scanning electron microscopy images were obtained respectively, as shown in FIG. 3, FIG. 4, and FIG. 5. The comparison shows that the dispersibility of the catalyst product prepared in Example 1 is very good, and the catalyst products prepared in Comparative Example 1 and Comparative Example 2 both have a large amount of agglomeration.

The catalyst synthesis device and catalyst synthesis method proposed by the present invention can be applied to the following types of catalyst synthesis, including but not limited to platinum-carbon catalysts, platinum alloy catalysts, platinum core-shell structure catalysts, and non-platinum catalysts.

The technical features of the above-mentioned embodiments can be combined arbitrarily. In order to make the description concise, all possible combinations of the various technical features in the above-mentioned embodiments are not described. However, as long as there is no contradiction in the combination of these technical features, All should be considered as the scope of this specification.

The above-mentioned embodiments only express several embodiments of the present invention, and the descriptions are relatively specific and detailed, but they should not be understood as limiting the scope of the invention patent. It should be pointed out that for those of ordinary skill in the art, without departing from the concept of the present invention, several modifications and improvements can be made, and these all fall within the protection scope of the present invention. Therefore, the protection scope of the patent of the present invention should be subject to the appended claims.

Claims

A continuous decentralized system, characterized in that it includes:

Ultrasonic module, the power of the ultrasonic module is not less than 500W, used to disperse materials;

Stirring module for dispersing materials; and

The material circulation mechanism connects the ultrasonic module with the stirring module, so that the materials in the ultrasonic module and the stirring module can circulate and circulate with each other.
The continuous dispersion system according to claim 1, wherein the ultrasonic module includes a material containing mechanism connected with the material circulation mechanism and at least a part of an ultrasonic mechanism arranged inside the material containing mechanism.
3. The continuous dispersion system according to claim 2, wherein the continuous dispersion system further comprises a heat dissipation mechanism for cooling and dissipating the ultrasonic module.
The continuous dispersion system according to claim 3, wherein the heat dissipation mechanism includes a cooling medium circulation pipeline and a cooling medium circulation pump arranged on the cooling medium circulation pipeline.
The continuous dispersion system of claim 4, wherein the cooling medium containing mechanism and the material containing mechanism are an integrated structure, and the material containing mechanism is a housing with a containing cavity, and the containing The cavity is used for accommodating materials for ultrasound. The housing includes an outer wall and an inner wall, and an interlayer space for accommodating a cooling medium is formed between the outer wall and the inner wall.
The continuous dispersion system according to claim 5, wherein the inner wall is further provided with a material circulation inlet and a material circulation outlet that are connected to the accommodating cavity and the material circulation mechanism, and the material circulation mechanism It is located at least partially within the interlayer space.
7. The continuous dispersion system according to any one of claims 1 to 6, wherein the continuous dispersion system comprises at least two of the ultrasonic modules, and each of the ultrasonic modules is connected in series.
The continuous dispersion system according to any one of claims 1 to 6, wherein the material circulation mechanism comprises a material circulation pump and a material circulation pipeline, and the material circulation pipeline is connected to the ultrasonic module and the Between the mixing modules, the material circulation pump is installed on the material circulation pipeline.
The continuous dispersion system according to any one of claims 1 to 6, wherein the power of the ultrasonic module is not less than 1000W.
A carbon carrier dispersion device, characterized in that it comprises an initial dispersion mechanism and the continuous dispersion system according to any one of claims 1-9, the material circulation mechanism is provided with an inlet, and the initial dispersion mechanism is connected to the continuous dispersion system. The feed inlet is connected.
A catalyst synthesis device, characterized in that it comprises the carbon carrier dispersion device according to claim 10, a reaction kettle and a catalyst collection device that are sequentially connected to the carbon carrier dispersion device, and a discharge port is provided on the material circulation mechanism , The discharge port of the material circulation mechanism is in communication with the reaction kettle.
A method for batch synthesis of catalysts, characterized in that the batch synthesis of catalysts using the catalyst synthesis device of claim 11 includes:

Cleaning and drying the catalyst synthesis device, adding a predetermined amount of solvent and carbon black to the preliminary dispersion mechanism, and turning on the stirring;

Stir for a predetermined time to form a suspension. When there is no obvious solid deposit at the bottom of the initial dispersion mechanism, open the feed inlet to allow the suspension to enter and fill the continuous dispersion system, close the feed inlet, and turn on the ultrasonic module, The stirring module and the material circulation mechanism make the material continuously circulate ultrasonically for a predetermined time in the continuous dispersion system to form a uniformly dispersed carbon carrier dispersion;

Open the discharge port, make the carbon carrier dispersion enter the reactor, add or pre-add the catalyst precursor material and the solvent at the same time, continue to stir, control the temperature, and start the catalyst synthesis reaction;

After the reaction is completed, the mixture in the reactor is introduced into the catalyst collection device and filtered to obtain the primary catalyst; and

The primary catalyst is subjected to post-treatment to obtain a catalyst product.