CN110639415A - Continuous dispersion system, catalyst batch synthesis device and method - Google Patents
Continuous dispersion system, catalyst batch synthesis device and method Download PDFInfo
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F33/00—Other mixers; Mixing plants; Combinations of mixers
- B01F33/80—Mixing plants; Combinations of mixers
- B01F33/82—Combinations of dissimilar mixers
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/18—Stationary reactors having moving elements inside
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/40—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals of the platinum group metals
- B01J23/42—Platinum
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- B01J35/23—
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
- B01J37/0201—Impregnation
- B01J37/0211—Impregnation using a colloidal suspension
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/34—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
- B01J37/341—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation
- B01J37/343—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation of ultrasonic wave energy
Abstract
The invention relates to a continuous dispersion system, a carbon carrier dispersion device, a catalyst synthesis device and a method, wherein the continuous dispersion system comprises a stirring module, an ultrasonic module, a material circulation mechanism and an ultrasonic module, wherein the power of the ultrasonic module is not lower than 500W and is used for dispersing materials; the stirring module is used for dispersing materials; and the material circulating mechanism is used for communicating the ultrasonic module with the stirring module so as to ensure that materials in the ultrasonic module and the stirring module can circulate mutually. Above-mentioned continuous dispersion system on the one hand through supersound module and stirring module common dispersed material keep the homodisperse of material in the continuous dispersion system, on the other hand through will stirring module and supersound module circulation, also accelerated nanometer superfine dispersion's heat conduction meanwhile, so the circulation is reciprocal for the big batch of material is dispersed and is gone on smoothly, and has improved the dispersion effect of big batch dispersion greatly, and then can improve the synthetic production efficiency of nano-material.
Description
Technical Field
The invention relates to the technical field of nano materials, in particular to a continuous dispersion system, a carbon carrier dispersion device, a catalyst synthesis device and a catalyst synthesis method.
Background
In the field of liquid-phase synthesis of nano materials, in order to avoid agglomeration of the nano materials, control of dispersion uniformity is always the core step of synthesis, and the performance of the materials is directly determined.
In the field of catalyst synthesis, the control of the dispersion uniformity of the nano material is more prominent. The improvement of catalytic performance of the catalyst is largely limited by the dispersibility of the material. Early in the development of catalyst materials, laboratory synthesis quantities were typically tens of milligrams, the amount of support material required was relatively small, and dispersion was relatively easy. However, in the mass production stage, the difficulty of controlling the dispersion uniformity is sharply increased. The dispersion control effect of the original laboratory is weakened, the requirements of improving the control conditions on the experimental environment and experimental equipment are greatly improved, meanwhile, the experimental risk is greatly increased, and the development difficulty of the batch production process is obviously increased. The prior art needs further improvement and optimization in the mass production technology of nano materials.
Disclosure of Invention
The present invention provides a continuous dispersion system, a carbon carrier dispersion device, a catalyst synthesis device, and a method, which can improve the dispersion effect of mass dispersion.
A continuous dispersion system comprising:
the power of the ultrasonic module is not lower than 500W, and the ultrasonic module is used for dispersing materials;
the stirring module is used for dispersing materials;
and the material circulating mechanism is used for communicating the ultrasonic module with the stirring module so as to ensure that materials in the ultrasonic module and the stirring module can circulate mutually.
Above-mentioned continuous dispersion system on the one hand through supersound module and stirring module common dispersed material keep the homodisperse of material in the continuous dispersion system, on the other hand will stir module and supersound module circulation through material circulation mechanism, make through stirring the module and refine even material can get into the supersound module and further the superfine dispersion, and the material that further the superfine dispersion was gone on through the supersound module also can get into the stirring module and further refine evenly, meanwhile also accelerated the thermal conduction of superfine dispersion, so circulation is reciprocal, make the big batch of material disperse smoothly, and improved the dispersion effect of big batch dispersion greatly, and then can improve the synthetic production efficiency of nano-material.
In some of these embodiments, the ultrasonic module includes a material containment mechanism in communication with the material circulation mechanism and an ultrasonic mechanism at least partially disposed within the material containment mechanism.
In some embodiments, the continuous dispersion system further comprises a heat dissipation mechanism for cooling and dissipating heat of the ultrasound module.
In some embodiments, the heat dissipation mechanism includes a cooling medium circulation line and a cooling medium circulation pump disposed on the cooling medium circulation line.
In some embodiments, the heat dissipation mechanism further comprises a cooling medium accommodating mechanism arranged outside the material accommodating mechanism, so that the outside of the material accommodating mechanism can be immersed in the cooling medium of the cooling medium accommodating mechanism, and the cooling medium accommodating mechanism is communicated with the cooling medium circulation pipeline in series.
In some embodiments, the cooling medium accommodating mechanism and the material accommodating mechanism are integrated, the material accommodating mechanism is a housing having an accommodating cavity, the accommodating cavity is used for accommodating materials for ultrasonic processing, 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 embodiments, the inner wall is further provided with a material circulation inlet and a material circulation outlet which are communicated 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 these embodiments, the continuous dispersion system includes at least two of the ultrasonic modules, each communicating in series.
In some embodiments, the material circulation mechanism includes a material circulation pump and a material circulation pipeline, the material circulation pipeline is communicated between the ultrasonic module and the stirring module, and the material circulation pump is installed on the material circulation pipeline.
In some embodiments, the material circulation mechanism further comprises a first control valve and a second control valve, the first control valve is arranged on the material circulation pipeline between one end of the ultrasonic module and the stirring module communicated with the ultrasonic module, and the second control valve is arranged on the material circulation pipeline between the other end of the ultrasonic module and the stirring module communicated with the ultrasonic module.
In some of these embodiments, the power of the ultrasound module is not less than 1000W.
A carbon carrier dispersing device comprises a primary dispersing mechanism and any one of the continuous dispersing systems, wherein a feeding opening is formed in a material circulating mechanism, and the primary dispersing mechanism is communicated with the feeding opening.
In some of these embodiments, the primary dispersing mechanism is a high speed shearing device.
A catalyst synthesis device comprises the carbon carrier dispersion device, a reaction kettle and a catalyst collection device, wherein the reaction kettle and the catalyst collection device are sequentially communicated with the carbon carrier dispersion device, a material circulation mechanism is provided with a discharge hole, and the discharge hole of the material circulation mechanism is communicated with the reaction kettle.
A catalyst batch synthesis method for synthesizing catalysts in batches by using the catalyst synthesis device comprises the following steps:
cleaning and drying the catalyst synthesis device, adding a predetermined amount of solvent and carbon black into the primary dispersing mechanism, and starting stirring;
stirring for a preset time to form a suspension, starting a material inlet when no obvious solid precipitate exists at the bottom of the primary dispersing mechanism, enabling the suspension to enter and fill the continuous dispersing system, closing the material inlet, and starting an ultrasonic module, a stirring module and a material circulating mechanism to enable the material to continuously circulate for ultrasonic preset time in the continuous dispersing system to form uniformly dispersed carbon carrier dispersion liquid;
opening a discharge port, enabling the carbon carrier dispersion liquid to enter a reaction kettle, simultaneously adding or pre-adding a catalyst precursor material and a solvent, continuously stirring, controlling the temperature, and starting a catalyst synthesis reaction;
after the reaction is finished, introducing the mixture in the reaction kettle into a catalyst collecting device, and filtering to obtain a primary catalyst; and
and carrying out post-treatment on the primary catalyst to obtain a catalyst product.
The catalyst synthesis process provided by the invention can be used for large-scale continuous production, and the obtained catalyst product has high dispersion uniformity.
Drawings
FIG. 1 is a schematic diagram of a continuous dispersion system according to an embodiment;
FIG. 2 is a schematic structural view of a catalyst synthesis apparatus according to an embodiment;
FIG. 3 is a scanning electron micrograph of the catalyst product obtained in example 1;
FIG. 4 is a scanning electron micrograph of the catalyst product prepared in comparative example 1;
FIG. 5 is a scanning electron micrograph of the catalyst product prepared in comparative example 2.
Detailed Description
To facilitate an understanding of the invention, the invention will now be described more fully with reference to the accompanying drawings. Preferred embodiments of the present invention are shown in the drawings. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
It will be understood that when an element is referred to as being "secured to" another element, it can be directly on the other element or intervening elements may also be present. When an element is referred to as being "connected" to another element, it can be directly connected to the other element or intervening elements may also be present.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
The skilled artisan has found that the use of high shear emulsification alone to disperse large batches of carrier materials does not allow the dispersion of agglomerated nanoscale materials to the nanoscale level. If the ultrasonic device is used alone, only small batches of agglomerated nano-scale materials can be dispersed to the nano-scale; if dispersed in bulk, a large amount of heat is generated, and highly reactive support materials (e.g., carbon support materials) are extremely unsafe and explosive after a large amount of heat is generated. In addition, the ultrasonic device for nano-grade crushing has higher power, brings noise and heat generation, and further increases the difficulty of mass dispersion. The problem of ultrasonic efficiency still exists in the ultrasonic dispersion of big batch high power, and how effectively to utilize ultrasonic energy, it is urgent need to solve to improve ultrasonic efficiency.
Referring to fig. 1, an embodiment of the present invention provides a continuous dispersion system 100, which includes a stirring module 110, an ultrasonic module 120, and a material circulation mechanism (not shown).
The stirring module 110 is used for dispersing the materials, so that the materials can keep uniform dispersion in the flow, and the ultrasonic effect loss caused by agglomeration is avoided. The power of the ultrasonic module 120 is 1200W, and the ultrasonic module is used for performing high-power ultrasonic dispersion on the materials.
The material circulation mechanism is used for communicating the stirring module 110 with the ultrasonic module 120, so that materials in the stirring module 110 and the ultrasonic module 120 can be circulated mutually to form a flowing dispersion system. The flow dispersion system provided by the invention is beneficial to circulating multiple times of ultrasound, and the ultrasound efficiency is improved; meanwhile, the heat generated by the ultrasound is taken out, and the heat is reduced to be accumulated in the ultrasound module, so that danger is caused.
The continuous dispersion system 100 can keep the uniform dispersion of the materials in the continuous dispersion system 100 by jointly dispersing the materials through the ultrasonic module 120 and the stirring module 110, and can circulate the stirring module 110 and the ultrasonic module 120 through the material circulation mechanism, so that the materials refined and uniform through the stirring module 110 can enter the ultrasonic module 120 for further ultrafine dispersion, and the materials refined and further ultrafine dispersion through the ultrasonic module 120 can also enter the stirring module 110 for further refining and uniform, and meanwhile, the conduction of heat of ultrafine dispersion is accelerated, and the circulation is repeated, so that the large-batch dispersion of the materials is smoothly carried out, the dispersion effect of the large-batch dispersion is greatly improved, and the production efficiency of nano material synthesis can be improved.
The invention is mainly characterized in that the overall design of a continuous dispersion system is provided, and the overall design scheme is provided by fully considering the factors of dispersion uniformity formation, dispersion uniformity control, heat dispersion, continuous production and the like.
In particular, the use of the continuous dispersion system 100 described above can be used to disperse large batches of nanoscale support materials, such as nanoscale carbon materials.
In some examples, the stirring module 110 is a magnetic stirring module or a mechanical stirring module. In one particular example, the stirring module 110 is a magnetic stirrer.
In other examples, the agitation module 110 is an ultrasonic agitator 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 containment mechanism 121 in communication with the material circulation mechanism and an ultrasonic mechanism 122 at least partially disposed within the material containment mechanism. The ultrasonic mechanism 122 is used for generating ultrasonic waves to perform high-power ultrasonic dispersion on the material in the material containing mechanism 121. The material accommodating 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 the ultrasonic modules 120 is multiple (more than two), the plurality of ultrasonic modules 120 are connected in series, and each ultrasonic module 120 and the stirring module 110 are connected by a material circulation mechanism. Thus, a multistage dispersion system is formed by the plurality of ultrasonic modules 120, and the nano-scale dispersion effect can be further improved. In addition, the multi-stage ultrasound decentralized system may also reduce the ultrasound power of the ultrasound module 120.
For example, in one particular example, the ultrasound module 120 is an ultrasound device or an ultrasonic disperser.
It will be appreciated that the ultrasonic apparatus, in addition to comprising the material containment means 121 and the ultrasonic means 122, also has an ultrasonic horn, preferably of low power, which, by providing a multi-stage ultrasonic apparatus, can be used to perform hectogram batch carbon material processing.
Further, the number of the ultrasound modules 120 is plural, and the plural ultrasound modules 120 are sequentially disposed adjacently.
In some embodiments, the continuous dispersion system 100 further includes a heat dissipation mechanism for cooling and dissipating the ultrasonic module 120, so as to further reduce the risk of explosion due to the heat accumulation of the nano-scale ultra-fine dispersion of the material.
Further, the heat dissipation mechanism includes a cooling medium circulation pump (not shown) and a cooling medium circulation pipeline 141, the cooling medium circulation pipeline 141 is used for cooling the ultrasonic module 120, and the cooling medium circulation pump is installed on the cooling medium circulation pipeline 141.
The cooling medium circulation line 141 is used for storing and circulating a cooling medium, such as cooling water.
When the number of the ultrasonic modules 120 is plural, the heat dissipation mechanism may simultaneously dissipate heat of the plural ultrasonic modules 120.
Further, the heat dissipation mechanism further comprises a cooling medium accommodating mechanism 142 arranged outside the material accommodating mechanism 121, so that the outside of the material accommodating mechanism 121 can be immersed in the cooling medium of the cooling medium accommodating mechanism 142, and the cooling medium accommodating mechanism 142 is communicated with the cooling medium circulation pipeline 141 in series, so that the cooling medium is circulated, and thus the heat dissipation effect can be further improved.
In a specific embodiment, as shown in fig. 1, the ultrasonic module 120 includes 3 serially connected ultrasonic dispersers, each of which has a power of 500-.
In a preferred embodiment, the ultrasound module 120 and the agitation module 110 are spaced apart in a continuous dispersion system, for example, the number of the ultrasound module 120 and the agitation module 110 is 3. The materials sequentially flow 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, the power of each ultrasonic module 120 is not lower than 800W, and then the materials flow into a reaction kettle of the catalyst synthesis device through a discharge hole.
Further, the heat dissipation mechanism and the ultrasonic dispersion instrument are integrated devices. The material accommodating mechanism 121 in the ultrasonic dispersion instrument is a shell with an accommodating cavity. The holding chamber is used for holding materials for ultrasonic treatment, the shell comprises an outer wall and an inner wall, and an interlayer space for holding a cooling medium is formed between the outer wall and the inner wall. The housing with the intermediate space thus also corresponds to the cooling medium receiving means 142 of the heat dissipation means. In other words, the cooling medium accommodating unit 142 of the heat dissipating unit and the material accommodating unit 121 of the ultrasonic module are integrated.
Specifically, the outer wall is also provided with a cooling medium inlet and a cooling medium outlet so as to enable the cooling medium to be communicated in the interlayer space.
Specifically, a material circulation inlet and a material circulation outlet which are communicated with the accommodating cavity and the material circulation mechanism are further arranged on the inner wall, so that materials are circularly communicated among the material accommodating mechanism 121, the material circulation mechanism and the stirring module 110.
Specifically, at least part of the material circulating mechanism is positioned in the interlayer space. The cooling medium in the interlayer space can cool and radiate the materials in the accommodating cavity and can cool and radiate the materials in the material circulating mechanism.
Specifically, a material circulation pipeline 131 (see below) of the material circulation mechanism passes through an interlayer space formed by the outer wall and the inner wall of the housing and is respectively communicated with a material circulation inlet and a material circulation outlet on the inner wall, so that materials in the material circulation pipeline 131 are communicated with materials in the accommodating cavity. The cooling medium in the interlayer space can cool and radiate the materials in the accommodating cavity and can cool and radiate the materials in the material circulating pipeline 13. In some embodiments, the material circulation mechanism includes a material circulation pump (not shown) and a material circulation pipeline 131, the material circulation pipeline 131 is connected between the ultrasonic module 120 and the stirring module 110, and the material circulation pump is installed on the material circulation pipeline 131. Thus, the circulation of the material between the ultrasonic module 120 and the stirring module 110 is realized through the material circulation pump and the material circulation pipeline 131.
Further, the material circulation mechanism further includes a first control valve 132 and a second control valve 133. The first control valve 132 is disposed on the material circulation line 131 between one end of the ultrasonic module 120 and the stirring module 110 communicated therewith. The second control valve 133 is disposed on the material circulation line 131 between the other end of the ultrasonic module 120 and the stirring module 110 communicated therewith. The flow of material is thus controlled by the two control valves.
Wherein one end and the other end of the stirring module 110 are the two ends of the stirring module 110 and the material circulation pipeline 131. Specifically, one end of the material circulation pipeline 131 is used for feeding the material into the stirring module 110, and the other end of the material circulation pipeline 131 is used for feeding the material from the stirring module 110.
Further, in the continuous dispersing system 100, the material inlet may be disposed at the stirring module 110 or the ultrasonic module 120, and the material is first added into the stirring module 110 or the ultrasonic module 120 and then circulated among the dispersing mechanisms through the material circulating mechanism. In this example, the material inlet is disposed on the stirring module 110.
An embodiment of the present invention also provides a carbon carrier dispersion device of an embodiment, including the preliminary dispersion mechanism and any one of the above continuous dispersion systems. Wherein, a material circulating mechanism in the continuous dispersion system is provided with a material inlet, and the primary dispersion mechanism is communicated with the material inlet.
In one particular example, the primary dispersion mechanism is a high speed shearing device, such as a high speed shearing emulsifier. It is understood that the primary dispersion mechanism is not limited thereto, and may be another homogenizer.
Referring to fig. 1 and 2, an embodiment of the present invention further provides a catalyst synthesis apparatus 10 including a continuous dispersion system 100, a reaction vessel 200, and a catalyst collection device 300, which are connected in sequence. And a discharge hole 1301 is formed in the material circulating mechanism, and the discharge hole of the material circulating mechanism is communicated with the reaction kettle 200.
Further, the discharge hole 1301 of the material circulation pipeline 131 is used for discharging the materials dispersed by the continuous dispersion system 100. Further, in order to control the opening and closing of the discharge hole 1301, a third control valve (not shown) may be provided at the discharge hole.
Wherein, reaction kettle 200 is used for the material reaction to obtain the catalyst, and catalyst collection device 300 is used for collecting the catalyst.
Specifically, continuous dispersion system 100 is in communication with reaction vessel 200 through outlet port 1301.
Further, the catalyst collecting device 300 is a filtering device, and the catalyst collecting device 300 is disposed at an outlet end of the discharging pipeline of the reaction kettle 200.
Specifically, the catalyst collecting device 300 includes a collecting funnel (not shown) installed at an outlet end of the discharging pipe of the reaction kettle 200, and a filter screen (not shown) installed on the collecting funnel for filtering the liquid phase and collecting the solid phase, i.e., the catalyst. The catalyst synthesizing apparatus 10 further includes a first waste collecting device 400 for collecting the liquid-phase waste liquid filtered by the catalyst collecting device 300.
Further, the catalyst synthesis apparatus 10 further includes a second waste collection device 500, and the second waste collection device 500 is connected to the reaction kettle 200 and is used for collecting the waste liquid in the reaction kettle 200.
The continuous dispersion system 100 described above may be used for dispersion of support materials in catalyst synthesis, such as nanoscale carbon support materials. The catalyst synthesis apparatus 10 can be used for catalyst synthesis, and can synthesize 200g or more of catalyst in a single batch and 400g or more of catalyst per day.
Accordingly, a method for material dispersion using the continuous dispersion system 100 or a method for catalyst synthesis using the catalyst synthesis apparatus 10 is provided.
An embodiment of the present invention further provides a batch synthesis method of a catalyst according to an embodiment, where the catalyst synthesis apparatus is used to synthesize a catalyst in a batch, the batch synthesis method of a catalyst including the steps of:
step 1: the catalyst synthesis apparatus is cleaned, dried, added with a predetermined amount of solvent and carbon black into the primary dispersion mechanism, and stirred.
Step 2: stirring for a preset time to form turbid liquid, starting the material inlet when no obvious solid precipitate exists at the bottom of the primary dispersing mechanism, enabling the turbid liquid to enter and fill the continuous dispersing system, closing the material inlet, and starting the ultrasonic module, the stirring module and the material circulating mechanism to enable the materials to continuously circulate for ultrasonic preset time in the continuous dispersing system to form uniformly dispersed carbon carrier dispersion liquid.
And step 3: opening a discharge port, enabling the carbon carrier dispersion liquid to enter a reaction kettle, simultaneously adding or pre-adding a catalyst precursor material and a solvent, continuously stirring, controlling the temperature, and starting a catalyst synthesis reaction.
And 4, step 4: and after the reaction is finished, introducing the mixture in the reaction kettle into a catalyst collecting device, and filtering to obtain the primary catalyst.
And 5: and carrying out post-treatment on the primary catalyst to obtain a catalyst product.
In one embodiment, the catalyst precursor material, the reducing agent and the carbon-dispersing carrier passed through the continuous dispersion system are separately caused to flow to the catalyst reaction vessel, and the compounding ratio of the reaction material is controlled by controlling the flow rates of the carbon-dispersing carrier, the catalyst precursor material and the reducing agent into the reaction vessel.
To better illustrate the benefits of the continuous dispersion system, the following is a specific example of the use of the continuous dispersion system 100 for material dispersion.
Detailed description of the preferred embodiment 1
The catalyst synthesis apparatus shown in fig. 2 is used, which includes a continuous dispersion system 100, a reaction vessel 200, a catalyst collecting apparatus 300, a first waste collecting apparatus 400, a second waste collecting apparatus 500, and a preliminary dispersion apparatus (not shown). Wherein continuous dispersion system 100 is shown in figure 1. Wherein, the stirring module 110 is a magnetic stirrer, and the ultrasonic module 120 is a 1200W ultrasonic instrument. The primary dispersing device is a telling shearing emulsifying device, is connected with a feeding port of the continuous dispersing system and is controlled to be switched through a valve.
Step 1: and cleaning and drying the catalyst synthesis device. The first control valve 132 and the second control valve 133 were in a closed state, and 5L of the solvent (H) was added to the high-shear emulsifier2O), 10g of carbon black (EC300J, Lion) is weighed out and put into a high-speed shearing emulsifying machine, and stirring is started.
Step 2: stirring the materials in the high-speed shearing emulsifying machine for 30min to form a suspension, and starting a feeding port of the continuous dispersing system when no obvious solid precipitate exists at the bottom of the high-speed shearing emulsifying machine so as to enable the materials to enter the continuous dispersing system. And opening the first control valve 132 and the second control valve 133 to enable the suspension to flow to each ultrasonic module 120 through the material circulation mechanism, and starting the ultrasonic device after the material flows stably. After 30 minutes of sonication, the liquid in the sonication device was confirmed to be free of significant suspended particles. If suspended particles exist, the first control valve 132 and the second control valve 133 are opened to continue entering the high-speed shearing emulsifying machine to start stirring, and the operation is repeated in a circulating mode until the liquid in the ultrasonic device is free of obvious suspended particles.
And step 3: and opening a third control valve to open a discharge port, and introducing the suspension into an ultrasonic device between the continuous dispersion system and the reaction kettle for further dispersion.
And 4, step 4: and then introducing the suspension into a reaction kettle, continuously stirring, controlling the temperature, and adding platinum salt and a reducing agent with preset mass for reaction. After reacting for 1 hour, the mixture in the reaction kettle is introduced into a catalyst collecting device and filtered to obtain a primary catalyst.
And 5: and carrying out post-treatment on the primary catalyst to obtain a catalyst product.
Comparative example 1
Comparative example 1 Dispersion of 10g of carbon black in 5L of solvent (H) using high shear emulsification alone2O), adding the obtained suspension into a single 200W ultrasonic disperser for dispersing for 1h, and transferring the ultrasonically dispersed liquidMoving the mixture into a reaction kettle, continuously stirring, controlling the temperature, and adding platinum salt and a reducing agent with preset mass for reaction. After reacting for 1 hour, the mixture in the reaction kettle is introduced into a catalyst collecting device and filtered to obtain a primary catalyst. And carrying out post-treatment on the primary catalyst to obtain a catalyst product.
Comparative example 2
Comparative example 2 Dispersion of 10g of carbon Black in 5L of solvent (H) Using high shear emulsification alone2And O), transferring the dispersion liquid after ultrasonic treatment to a reaction kettle, continuously stirring, controlling the temperature, and adding platinum salt and a reducing agent with preset mass for reaction. After reacting for 1 hour, the mixture in the reaction kettle is introduced into a catalyst collecting device and filtered to obtain a primary catalyst. And carrying out post-treatment on the primary catalyst to obtain a catalyst product.
The catalyst products prepared in example 1, comparative example 1 and comparative example 2 were subjected to scanning transmission electron microscopy characterization to obtain scanning electron microscopy images, as shown in fig. 3, fig. 4 and fig. 5, respectively. As can be seen by comparison, the catalyst products prepared in example 1 have very good dispersibility, and the catalyst products prepared in comparative example 1 and comparative example 2 have a large amount of agglomeration.
The catalyst synthesis device and the catalyst synthesis method provided by the invention can be applied to the synthesis of the following catalysts, 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 embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (12)
1. A continuous dispersion system, comprising:
the power of the ultrasonic module is not lower than 500W, and the ultrasonic module is used for dispersing materials;
the stirring module is used for dispersing materials; and
and the material circulating mechanism is used for communicating the ultrasonic module with the stirring module so as to ensure that materials in the ultrasonic module and the stirring module can circulate mutually.
2. The continuous dispersion system of claim 1, wherein the ultrasonic module comprises a material containment mechanism in communication with the material circulation mechanism and an ultrasonic mechanism disposed at least partially within the material containment mechanism.
3. The continuous dispersion system of claim 2, further comprising a heat sink mechanism for cooling and dissipating heat from the ultrasound module.
4. A continuous dispersion system according to claim 3, wherein said heat radiating mechanism includes a cooling medium circulating line and a cooling medium circulating pump provided on said cooling medium circulating line.
5. The continuous dispersing system of claim 4, wherein the cooling medium receiving mechanism and the material receiving mechanism are an integrated structure, the material receiving mechanism is a housing having a receiving cavity for receiving the material for ultrasonic processing, the housing includes an outer wall and an inner wall, and an interlayer space for receiving the cooling medium is formed between the outer wall and the inner wall.
6. A continuous dispersion system according to claim 5 wherein the inner wall is further provided with a material circulation inlet and a material circulation outlet communicating with the chamber and the material circulation means, at least part of the material circulation means being located in the plenum space.
7. A continuous dispersion system according to any one of claims 1 to 6 wherein the continuous dispersion system comprises at least two said ultrasonic modules, each of said ultrasonic modules being in series communication.
8. The continuous dispersing system of any one of claims 1 to 6, wherein the material circulating mechanism comprises a material circulating pump and a material circulating pipeline, the material circulating pipeline is communicated between the ultrasonic module and the stirring module, and the material circulating pump is installed on the material circulating pipeline.
9. A continuous dispersion system according to any one of claims 1 to 6 wherein the power of the ultrasonic module is not less than 1000W.
10. A carbon carrier dispersing device is characterized by comprising a primary dispersing mechanism and the continuous dispersing system as claimed in any one of claims 1 to 9, wherein a material inlet is formed in the material circulating mechanism, and the primary dispersing mechanism is communicated with the material inlet.
11. A catalyst synthesis device, which is characterized by comprising the carbon carrier dispersion device of claim 10, and a reaction kettle and a catalyst collection device which are sequentially communicated with the carbon carrier dispersion device, wherein a material outlet is arranged on the material circulation mechanism, and the material outlet of the material circulation mechanism is communicated with the reaction kettle.
12. A method for batch synthesis of a catalyst, which comprises the step of using the catalyst synthesis apparatus according to claim 11 to synthesize a catalyst in a batch manner, comprising:
cleaning and drying the catalyst synthesis device, adding a predetermined amount of solvent and carbon black into the primary dispersing mechanism, and starting stirring;
stirring for a preset time to form a suspension, starting a material inlet when no obvious solid precipitate exists at the bottom of the primary dispersing mechanism, enabling the suspension to enter and fill the continuous dispersing system, closing the material inlet, and starting an ultrasonic module, a stirring module and a material circulating mechanism to enable the material to continuously circulate for ultrasonic preset time in the continuous dispersing system to form uniformly dispersed carbon carrier dispersion liquid;
opening a discharge port, enabling the carbon carrier dispersion liquid to enter a reaction kettle, simultaneously adding or pre-adding a catalyst precursor material and a solvent, continuously stirring, controlling the temperature, and starting a catalyst synthesis reaction;
after the reaction is finished, introducing the mixture in the reaction kettle into a catalyst collecting device, and filtering to obtain a primary catalyst; and
and carrying out post-treatment on the primary catalyst to obtain a catalyst product.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111185120A (en) * | 2020-01-09 | 2020-05-22 | 吕梁学院 | High-efficient dispersion dosing unit of graphite alkene production usefulness |
| CN114177858A (en) * | 2021-12-13 | 2022-03-15 | 清氢(北京)科技有限公司 | Large-scale preparation method and large-scale preparation device of electrocatalyst |
| CN115872734A (en) * | 2022-10-27 | 2023-03-31 | 先导薄膜材料（广东）有限公司 | ITO powder reproduced from ITO waste target, high-density target and preparation method thereof |
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| KR101282118B1 (en) * | 2011-01-24 | 2013-07-03 | 엄재홍 | Oil and water Agitator |
| CN102423545A (en) * | 2011-10-21 | 2012-04-25 | 北京弘祥隆生物技术股份有限公司 | Ultrasonic crystallizing equipment used in natural product or chemical agent crystallization and purification |
| CN206045913U (en) * | 2016-06-29 | 2017-03-29 | 昆明纳太科技有限公司 | The equipment of continuous dispersion nano material |
| CN106058272A (en) * | 2016-07-25 | 2016-10-26 | 北京工业大学 | Environmentally friendly one-step synthesis method of small-grain-size uniformly dispersed noble metal nanoparticle electro-catalyst |
| CN206911273U (en) * | 2017-06-16 | 2018-01-23 | 北京华科讯能石墨烯新技术研究院有限公司 | Graphene peels off tri compound plant equipment |
| CN208865563U (en) * | 2018-08-09 | 2019-05-17 | 扬州北方三山工业陶瓷有限公司 | A kind of new type ultrasonic Ball-stirring mill combined cycle pulping device |
| CN208786191U (en) * | 2018-08-23 | 2019-04-26 | 湖南金华达建材有限公司 | It is a kind of for producing the high-performance device of concrete parting agent |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111185120A (en) * | 2020-01-09 | 2020-05-22 | 吕梁学院 | High-efficient dispersion dosing unit of graphite alkene production usefulness |
| CN114177858A (en) * | 2021-12-13 | 2022-03-15 | 清氢(北京)科技有限公司 | Large-scale preparation method and large-scale preparation device of electrocatalyst |
| CN114177858B (en) * | 2021-12-13 | 2023-06-16 | 清氢(北京)科技有限公司 | Electrocatalyst macro preparation method and macro preparation device |
| CN115872734A (en) * | 2022-10-27 | 2023-03-31 | 先导薄膜材料（广东）有限公司 | ITO powder reproduced from ITO waste target, high-density target and preparation method thereof |
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Effective date of registration: 20200519 Address after: 318, building 4, No. 187, Jinshui Road, Licang District, Qingdao City, Shandong Province Applicant after: Qingdao chuangqixinneng Catalysis Technology Co., Ltd Address before: 215000 7 D building, 398 Shui Shui Road, Suzhou Industrial Park, Jiangsu Applicant before: SUZHOU TIANJI INNOVATION NANO TECHNOLOGY Co.,Ltd. |