CN110639409A - Method and device for preparing homogeneous catalyst slurry with controllable concentration - Google Patents
Method and device for preparing homogeneous catalyst slurry with controllable concentration Download PDFInfo
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- CN110639409A CN110639409A CN201910877857.4A CN201910877857A CN110639409A CN 110639409 A CN110639409 A CN 110639409A CN 201910877857 A CN201910877857 A CN 201910877857A CN 110639409 A CN110639409 A CN 110639409A
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- 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
- B01F33/70—Mixers specially adapted for working at sub- or super-atmospheric pressure, e.g. combined with de-foaming
- B01F33/71—Mixers specially adapted for working at sub- or super-atmospheric pressure, e.g. combined with de-foaming working at super-atmospheric pressure, e.g. in pressurised vessels
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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
- B01F23/00—Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
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Abstract
The invention provides a preparation method and a device of homogeneous catalyst slurry with controllable concentration. The preparation method of the homogeneous catalyst slurry with controllable concentration comprises the following steps: the method comprises the steps of stirring the catalyst in a vacuum container until the catalyst is completely splashed and is in a dust-raising shape; injecting water mist into the container to fully wet the catalyst; injecting preset ingredients into the container, and uniformly mixing the ingredients with the catalyst to obtain slurry; and step four, homogenizing the slurry. In an oxygen-free vacuum container, firstly, the combination of the catalyst and atomized water is completed, the wetting of the catalyst is realized, and the oxidation of the catalyst is avoided; and in addition, in the process of uniformly mixing other auxiliary materials with the catalyst, volatilization loss is not easy to occur, the stability of the slurry concentration is realized, and the homogenization of the catalyst is further ensured.
Description
Technical Field
The invention belongs to the technical field of catalysts, and particularly relates to a preparation method and a device of homogeneous catalyst slurry with controllable concentration.
Background
Proton Exchange Membrane Fuel Cells (PEMFCs) have the advantages of high power density, low-temperature operation, cleanliness, no pollution, and the like, are efficient, reliable, environment-friendly, and are receiving more and more attention from many countries. The Membrane Electrode (MEA) is the most important component part of PEMFC, and it is not only an important site for electron generation and separation, but also carries the transport of gas and product water, and has very important influence on the electrochemical performance of PEMFC.
The MEA preparation method may be classified into a conventional Gas Diffusion Electrode (GDE) method and a catalyst-coated membrane (CCM) method according to the catalyst slurry coating position. The GDE method generally prepares the catalyst in slurry onto the gas diffusion layer by coating, spraying, etc.; the CCM process is a process in which the catalyst and other additives in the catalyst slurry are prepared directly onto the proton exchange membrane. Whichever method is used to prepare the MEA involves the preparation of the catalyst slurry.
The catalyst slurry is prepared by dispersing an electrocatalyst for a fuel cell in a specific solvent and passing the dispersion through a homogenizing and dispersing apparatus to homogenize the slurry as much as possible. The higher the homogenization degree of the slurry is, the higher the dispersion degree of the catalyst particles in the slurry is, the more uniform the catalyst loading of different regions of the prepared CCM is, the higher the utilization rate of the catalyst is, the better the performance of different regions of the CCM and the consistency of the performance of different MEA are, and the factors are important for improving the performance and durability of the membrane electrode and reducing the cost of the membrane electrode. Therefore, catalyst slurry dispersion is a very important link in membrane electrode technology, and is directly related to the utilization rate of the catalyst and the performance of the membrane electrode.
The preparation method of the conventional catalyst slurry comprises the following steps: at room temperature, deionized water, a high molecular polymer proton conductor solution, a Polytetrafluoroethylene (PTFE) solution, alcohol, a thickener and the like are sequentially added into catalyst particles, and then a shear emulsifying machine, an ultrasonic dispersion machine and other dispersion equipment are used for homogenizing the slurry, so that the catalyst slurry required by the preparation of the membrane electrode is finally obtained.
The catalyst used for preparing the membrane electrode has high activity, and can be directly exposed in the air to cause oxidation reaction which is difficult to be found by naked eyes, so that the catalyst is partially oxidized and loses certain catalytic activity; in addition, although a certain amount of deionized water is added into the catalyst particles in the first step when the slurry is dispersed, mainly in order to prevent the catalyst particles from being oxidized in a large probability due to contact with an organic solvent in an air atmosphere and even from spontaneously combusting in extreme cases, simply adding a certain amount of deionized water dropwise onto the surfaces of the catalyst particles cannot completely ensure that all the catalyst particles are wetted by water to achieve the effect of isolating air, and under the condition, if the organic solvent is added into the catalyst particles, part of the catalyst which is not wetted is oxidized, so that the catalyst is partially deactivated; in addition, in the conventional dispersing device, the catalyst slurry and the slurry container are directly communicated with the air, and the volatile organic solvent in the slurry can be partially volatilized in the dispersing process, so that the concentration of the slurry is changed, namely the concentration is uncontrollable, the loading amount of the catalyst in the membrane electrode is directly uncontrollable, and the performance and the consistency of the membrane electrode are not ensured.
Disclosure of Invention
Therefore, the technical problem to be solved by the present invention is to provide a method and an apparatus for preparing homogeneous catalyst slurry with controllable concentration, which can reduce the oxidation of the catalyst and stabilize the concentration.
In order to solve the above problems, the present invention provides a method for preparing a homogeneous catalyst slurry with controllable concentration, comprising the steps of:
the method comprises the steps of stirring the catalyst in a vacuum container until the catalyst is completely splashed and is in a dust-raising shape;
injecting water mist into the container to fully wet the catalyst;
injecting preset ingredients into the container, and uniformly mixing the ingredients with the catalyst to obtain slurry;
and fourthly, homogenizing the slurry.
Preferably, the vessel is operated in an inert gas atmosphere.
Preferably, the weighing of the preset ingredients is carried out in an inert gas atmosphere.
Preferably, the injecting the water mist is spraying deionized water into the container through an atomizing device.
Preferably, the stirring speed is 120-3000 rpm.
Preferably, the homogenized slurry is tested, and if the homogenization degree is less than a preset degree, the slurry is refluxed to the container and then stirred, mixed and homogenized.
Preferably, in the second step, the step of injecting the water mist into the container is to spray the water mist into the container by pressurizing inert gas and deionized water.
According to another aspect of the present invention, there is provided a device for preparing a homogeneous catalyst slurry with controllable concentration, comprising a sealed tank and a homogenizer, wherein the sealed tank is provided with a liquid atomization inlet and a stirring device, and the bottom of the sealed tank is connected with the inlet of the homogenizer.
Preferably, the outlet of the homogenizer is connected with the upper part of the seal tank through a multi-way valve.
Preferably, two seal tanks are arranged and are connected with the inlet of the homogenizer through a three-way valve and a peristaltic pump in sequence.
The invention provides a preparation method of homogeneous catalyst slurry with controllable concentration, which comprises the following steps: the method comprises the steps of stirring the catalyst in a vacuum container until the catalyst is completely splashed and is in a dust-raising shape; injecting water mist into the container to fully wet the catalyst; injecting preset ingredients into the container, and uniformly mixing the ingredients with the catalyst to obtain slurry; and step four, homogenizing the slurry. In a vacuum container, firstly, the combination of the catalyst and atomized water is completed, the wetting of the catalyst is realized, and the oxidation of the catalyst is avoided; and in addition, in the process of uniformly mixing other auxiliary materials with the catalyst, the volatilization loss of the solvent is not easy to occur, the stability of the concentration of the slurry is realized, and the homogenization of the catalyst is further ensured.
Drawings
Fig. 1 is a schematic structural diagram of a device for preparing homogeneous catalyst slurry with controllable concentration according to an embodiment of the present invention.
The reference numerals are represented as:
1. sealing the tank; 1', sealing the tank; 11. a liquid atomization inlet; 12. a stirring device; 2. a peristaltic pump; 3. a high-pressure homogenizer; 4. a three-way valve; 5. a four-way valve; 6. a ball valve; 6', a ball valve.
Detailed Description
According to an embodiment of the present invention, a method for preparing a homogeneous catalyst slurry with controllable concentration comprises the following steps:
the method comprises the steps of stirring the catalyst in a vacuum container until the catalyst is completely splashed and is in a dust-raising shape;
injecting water mist into the container to fully wet the catalyst;
injecting preset ingredients into the container, and uniformly mixing the ingredients with the catalyst to obtain slurry;
and fourthly, homogenizing the slurry.
In the vacuum container, the catalyst powder is stirred, so that the catalyst powder is in a dust-raising state and is filled in the whole container, the wetting of the catalyst is realized to the maximum limit by injecting water mist into the container, the catalyst is prevented from being exposed and oxidized, the preset ingredients are conveniently injected into the container on the next step, the catalyst can be uniformly mixed into slurry, and the subsequent homogenization process is facilitated.
Wherein, the preset ingredients include: a proton conductor solution, a polytetrafluoroethylene solution, and an alcohol; the mass ratio of the use amount of each material is as follows: the catalyst is water, the proton conductor solution is polytetrafluoroethylene solution, and the alcohol is 1: 1-5: 4-10: 2-10: 20-200. The catalyst is common catalysts such as Pt/C, Pt alloy, the proton conductor solution is perfluorosulfonic acid type polymer (Nafion) solution with the concentration of 5 wt% -20 wt%, and the concentration of Polytetrafluoroethylene (PTFE) solution is 10 wt% -70 wt%; the alcohol is organic solvent such as ethanol, isopropanol, glycerol, tert-butanol, etc.
The particle size of the catalyst is 1-10 nm, or the catalyst is attached to carrier particles, the carrier is high-conductivity carbon black, mesoporous carbon, graphene, carbon nano tubes, titanium dioxide and the like, the particle size of the carrier particles is 30-1000 nm, and in order to ensure stirring, the catalyst particles can form a dust-raising shape, and the stirring speed is 120-3000 rpm.
To ensure that the catalyst is not oxidized, the vessel may be rendered oxygen-free, e.g., the vessel may be operated under an inert gas atmosphere. In addition, the weighing of each of the preset ingredients was also performed in an inert gas atmosphere.
The water mist is injected by spraying deionized water into the container through an atomizing device.
And detecting the homogenized slurry, and if the homogenization degree is less than the preset degree, refluxing the slurry to the container and then stirring and uniformly mixing the slurry, so that the whole homogenization effect can be improved.
In the step II, the water mist injected into the container is sprayed into the container by pressurizing inert gas and deionized water, and the inert gas atmosphere is adopted to ensure the generation of the water mist and avoid the oxidation of the catalyst.
The preparation method of the invention has the following advantages:
1. the operation is completed in inert atmosphere, so that the possible oxidation or spontaneous combustion phenomenon of the catalyst in the slurry preparation process is avoided to the maximum extent, and the activity utilization rate of the catalyst is stabilized.
2. Under the inert atmosphere, the deionized water atomization and the catalyst bulking are combined, so that the catalyst is wetted to the maximum extent, and the possibility of oxidizing the catalyst is further reduced.
3. The whole slurry preparation process is basically carried out in a sealed container or pipeline, so that volatilization of a part of volatile solvents in the slurry is avoided to the maximum extent, controllability of the concentration of the slurry is realized, and uniformity of catalyst loading capacity on the membrane electrode is further ensured.
Referring to fig. 1 in combination, according to an embodiment of the present invention, an apparatus for preparing a homogeneous catalyst slurry with controllable concentration includes a sealed tank 1, a peristaltic pump 2, and a high-pressure homogenizer 3, where the sealed tank 1 is provided with a liquid atomization inlet 11 and a stirring device 12, the bottom of the sealed tank 1 is connected to an inlet of the peristaltic pump 2, and an outlet of the peristaltic pump 2 is connected to an inlet of the high-pressure homogenizer 3.
Under the natural condition of room temperature, various reagents for preparing the catalyst slurry are weighed in advance, and the specifications of the two parts are the same. Each part comprises 10g of deionized water, 30g of 5 wt% Nafion solution, 10g of 40 wt% PTFE solution and 400g of isopropanol solvent.
And (3) placing the two weighed reagents in a glove box, and simultaneously placing a container containing the catalyst and a balance for weighing the mass of the catalyst in the glove box. Then using N2And air in the glove box is replaced, and various experimental operations in the glove box are ensured to be carried out under inert atmosphere. Two 60 wt% Pt/C catalysts were weighed using a balance, 5g each, and the weighed catalysts were placed in closed, sealed jars 1 and 1' with a stirring device, respectively.
Seal the seal pot 1 and 1', then vacuumize the seal pot, after the vacuumization is finished, start the stirring device 12, the catalyst can be bulked continuously under the action of the stirring device 12, and then the whole cavity is filled. Then, the manual spray gun was connected to the liquid atomization inlet 11 on the upper side of the seal pot, and the spray gun was started (the gas used for the spray gun was N)2) And spraying the atomized deionized water into the sealed tank filled with the catalyst, so that the catalyst is fully wetted.
30g of 5 wt% Nafion solution, 10g of 40 wt% PTFE solution, and 400g of isopropyl alcohol were injected into the seal pots 1 and 1', respectively. Throughout the process, the stirring device 12 is in operation.
The ball valve 6 below the seal pot 1 is opened while the ball valve 6 'below the seal pot 1' is kept closed. The a and c of the three-way valve 4 are communicated, so that the slurry in the seal pot 1 is connected to the inlet end of the high-pressure homogenizer 3 through the three-way valve 4 and the peristaltic pump 2, and the homogenization of the slurry in the seal pot 1 is realized through the action of the high-pressure homogenizer 3.
The slurry is connected to a four-way valve 5 after coming out of the high-pressure homogenizer 3, at the moment, a and d of the four-way valve 5 are communicated, and the slurry in the seal tank 1 is homogenized and then continuously output. When the slurry output in the seal pot 1 is completed, that is, no slurry is output from the output port, the three-way valve 4 is switched to communicate b and c of the three-way valve 4, and simultaneously the ball valve 6 is closed and the ball valve 6 'is opened, at this time, the slurry in the seal pot 1' starts homogenizing operation. The a and c of the four-way valve 5 are communicated, after the high-pressure homogenizer 3 acts, the slurry flows back to the sealing tank 1 'again, the opening and closing states of the ball valve 6' and the three-way valve 4 are kept unchanged, the slurry is homogenized again, and the homogenization effect is improved. And (3) communicating the a and the d of the four-way valve 5, outputting the slurry through the four-way valve 5 after the high-pressure homogenizer 3 acts again, and finishing the homogenization of all the slurry when no slurry is output.
The preparation device of the invention has the following advantages:
1. the use of the high-pressure homogenizer improves the homogenization effect of the slurry on one hand, and on the other hand, the homogenizer can realize continuous input and output of the slurry, which provides possibility for large-scale preparation of the slurry.
2. The device can be used for large-scale production, a plurality of sealed seal tanks are cascaded, and one or more high-pressure homogenizers are matched, so that the continuous preparation of the slurry can be realized, the continuous output of the homogenized slurry is realized, and the large-scale production is facilitated.
It is easily understood by those skilled in the art that the above embodiments can be freely combined and superimposed without conflict.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention. The above description is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, several modifications and variations can be made without departing from the technical principle of the present invention, and these modifications and variations should also be regarded as the protection scope of the present invention.
Claims (10)
1. A preparation method of homogeneous catalyst slurry with controllable concentration is characterized by comprising the following steps:
the method comprises the steps of stirring a catalyst in a vacuum container until the catalyst flies up and is in a dust-raising shape;
injecting water mist into the container to fully wet the catalyst;
injecting preset ingredients into the container, and uniformly mixing the ingredients with the catalyst to obtain slurry;
and fourthly, homogenizing the slurry.
2. The method of claim 1, wherein the container is operated in an inert gas atmosphere.
3. The method according to claim 1 or 2, wherein the weighing of the predetermined ingredients is performed in an inert gas atmosphere.
4. The method of claim 3, wherein the injecting the water mist is spraying deionized water into the vessel by an atomizing device.
5. The method according to claim 1, wherein the stirring speed is 120 to 3000 rpm.
6. The method according to claim 1, wherein the homogenized slurry is tested, and if the homogenization degree is less than a predetermined degree, the slurry is refluxed to the container and then stirred, homogenized and homogenized.
7. The method according to claim 1 or 4, wherein the step of injecting the water mist into the container is spraying the water mist into the container by pressurizing the water mist with inert gas and deionized water.
8. The device for preparing the homogeneous catalyst slurry with controllable concentration is characterized by comprising a sealed tank and a homogenizer (3), wherein the sealed tank is provided with a liquid atomization inlet (11) and a stirring device (12), and the bottom of the sealed tank is connected with an inlet of the homogenizer (3).
9. The apparatus according to claim 8, wherein the outlet of the homogenizer (3) is connected to the upper part of the seal pot via a multi-way valve.
10. A device according to claim 8 or 9, wherein there are two said sealed tanks, connected to the inlet of said homogenizer (3) in turn through a three-way valve (4) and a peristaltic pump (2).
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Cited By (2)
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| CN111871295A (en) * | 2020-07-29 | 2020-11-03 | 河北养元智汇饮品股份有限公司 | Homogenizer pressurizing system and pressurizing method thereof |
| CN114984824A (en) * | 2022-06-29 | 2022-09-02 | 郑州磨料磨具磨削研究所有限公司 | Material mixing method and material mixing device for uniformly mixing abrasive and bonding agent |
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