Emulsion catalyst reactor device

Abstract

The utility model discloses an emulsion catalyst reactor device, which relates to the technical field of chemical preparation reaction equipment and comprises a reaction container and a stirring device, and the stirring device consists of an upper stirring device and a lower stirring device which are independently arranged up and down and have opposite rotation directions. And the upper stirring device and the lower stirring device are separated by a separation net. According to the emulsion catalyst reactor device provided by the utility model, the upper stirring device and the lower stirring device which are opposite in rotating direction are used for concentrating a liquid medium in the reactor to the middle, and emulsion in the upper part and emulsion in the lower part are gathered and collided in the middle of the reactor; a separation net is further arranged in the middle of the reactor, the number of the separation net can be selected according to the size of needed emulsion drops, the emulsion is further differentiated in the middle, fine emulsion drops are finally formed and scattered from the two sides of the reactor, benign drop refining circulation is formed in the reactor, and the emulsion with finer emulsion drops is finally obtained.

Description

Technical Field

[0001] The utility model relates to the technical field of chemical preparation reaction equipment, and specifically relates to an emulsifying catalyst reactor device. Background Technique

[0002] Emulsification is a phenomenon in which a liquid is evenly dispersed in another immiscible liquid in the form of extremely tiny droplets. The common emulsification we see is water-oil emulsification. During the preparation of catalysts, emulsified catalysts can better contact the reactants in the water-oil biphasic system, thereby improving the catalytic activity. For example, a Ni / ZrO2 emulsion catalyst for catalytic hydrogenation upgrading of octanoic acid disclosed in CN112717939A can increase the conversion rate of octanoic acid from 53.2% to 73.3%. The existing emulsification reaction device is an ordinary stirring reactor, and the emulsion water droplets of the obtained emulsified catalyst are relatively thick, which is difficult to meet the reaction requirements. Therefore, in order to further improve the emulsification effect and obtain finer emulsion water droplets, the utility model further improves the catalyst emulsification reaction device. Content of the Utility Model

[0003] The utility model aims to provide an emulsifying catalyst reactor device to solve the technical problem that the emulsion water droplets of the emulsified catalyst obtained by the existing emulsification reaction device are relatively thick.

[0004] To achieve the above purpose, the technical solution adopted by the utility model is as follows:

[0005] An emulsifying catalyst reactor device includes a reaction vessel and a stirring device. The stirring device is composed of an upper stirring device and a lower stirring device that are independently arranged up and down and rotate in opposite directions. A partition net is provided between the upper stirring device and the lower stirring device.

[0006] In the emulsifying catalyst reactor provided by the utility model, the upper stirring device and the lower stirring device rotating in opposite directions concentrate the liquid medium in the reactor towards the middle. The emulsions in the upper and lower parts converge and collide in the middle of the reactor. A partition net (the mesh number of the partition net can be selected according to the required size of the emulsion droplets) is also provided in the middle, so that the emulsion is further differentiated in the middle, and finally forms fine emulsion droplets and spreads out from both sides of the reactor, forming a good droplet refinement cycle in the reactor, and finally obtaining an emulsion with finer emulsion water droplets.

[0007] Preferably, the partition net is a copper net. The copper net has stable properties, is not easy to react with general reactants, and has a relatively low price.

[0008] Further, the specification of the copper net is 50-150 meshes. Too large or too small mesh holes may affect the droplet refinement effect, and this range is more suitable.

[0009] Furthermore, the specification of the copper mesh is 100 mesh. Through experimental verification, with a mesh size of 100 mesh, the obtained emulsion has a better reaction catalytic effect.

[0010] Preferably, the rotating shafts of at least one of the upper stirring device and the lower stirring device are hollow shafts for ventilation. Air can be introduced into the emulsion through the hollow rotating shafts, which is beneficial to the emulsification reaction.

[0011] Further, the rotating shaft of the lower stirring device is a hollow shaft for ventilation. Through experimental verification, when introducing air from the lower end, the obtained emulsion has a better reaction catalytic effect.

[0012] Compared with the prior art, the present utility model has the following beneficial effects:

[0013] For the emulsification catalyst reactor device provided by the present utility model, the upper stirring device and the lower stirring device with opposite rotation directions concentrate the liquid medium in the reactor towards the middle. The emulsions in the upper and lower parts converge and collide in the middle of the reactor. A partition mesh is also provided in the middle (the mesh number of the partition mesh can be selected according to the required size of the emulsion droplets), so that the emulsion is further differentiated in the middle, and finally forms fine emulsion droplets and spreads out from both sides of the reactor, forming a benign droplet refinement cycle in the reactor, and finally obtaining an emulsion with finer emulsion water droplets. Description of the Drawings

[0014] Figure 1 It is the external view of the emulsification catalyst reactor device provided for Example 1;

[0015] Figure 2 It is the sectional view of the emulsification catalyst reactor device provided for Example 1;

[0016] Figure 3 It is the comparison chart of the catalytic effects of the emulsification catalysts prepared by the devices with different ventilation methods in the catalytic hydrogenation reaction of octanoic acid;

[0017] Figure 4 It is the comparison chart of the catalytic effects of the emulsification catalysts prepared by the devices with different copper meshes in the catalytic hydrogenation reaction of octanoic acid;

[0018] The reference numerals in the figures are respectively: 1, reaction vessel; 2, upper stirring shaft; 3, lower stirring shaft; 4, upper stirring blade; 5, lower stirring blade; 6, copper mesh. Detailed Embodiments

[0019] In order to enable those skilled in the art to better understand the technical solutions of the present utility model, the present utility model will be further described below in conjunction with each embodiment and the drawings. The implementation manners of the present utility model include but are not limited to the following embodiments.

[0020] Throughout the specification, unless otherwise specifically stated, the terms used herein shall be construed as having the meanings as commonly used in the art. Therefore, unless otherwise defined, all technical and scientific terms used herein have the same meanings as those generally understood by those skilled in the art to which this utility model belongs. In case of any contradiction, this specification shall prevail.

[0021] Unless otherwise specifically stated, various raw materials, reagents, instruments, equipment, etc. used in this utility model can be obtained through market purchase or can be prepared by existing methods.

[0022] Example 1

[0023] As Figure 1 , Figure 2 As shown, it is the emulsifying catalyst reactor device provided by this embodiment. The emulsifying catalyst reactor device includes a reaction vessel 1 and a stirring device composed of an upper stirring device and a lower stirring device. The upper stirring device and the lower stirring device are independently arranged up and down, rotate in opposite directions, and are separated by a copper mesh 6 between the upper stirring device and the lower stirring device. The upper stirring device is composed of an upper stirring shaft 2 and upper stirring blades 4 fixed on the upper stirring shaft 2, and the lower stirring device is composed of a lower stirring shaft 3 and lower stirring blades 5 fixed on the lower stirring shaft 3.

[0024] In this embodiment, the upper stirring blades 4 rotate clockwise, and the lower stirring blades 5 rotate counterclockwise, concentrating the liquid medium in the reactor towards the middle. The emulsions in the upper and lower parts converge and collide in the middle of the reactor. There is also a copper mesh 6 in the middle, enabling the emulsions to be further differentiated in the middle, finally forming fine emulsion droplets and spreading out from both sides of the upper stirring blades 4 and the lower stirring blades 5, and forming a benign droplet refinement cycle in the reaction vessel 1, ultimately obtaining an emulsion with finer emulsion water droplets.

[0025] In the setting of this embodiment, at least one of the upper stirring shaft 2 and the lower stirring shaft 3 is set as a hollow shaft for transporting external gas into the emulsification reaction system. That is, in actual reactions, there are 3 ventilation methods: A is ventilation through the upper stirring shaft 2, B is ventilation through the lower stirring shaft 3, and C is ventilation through both the upper stirring shaft 2 and the lower stirring shaft 3 simultaneously. In order to verify which ventilation method is the best, this embodiment prepares the emulsion Ni / ZrO2 catalyst according to the scheme disclosed in CN112717939A (the process of preparing the emulsion Ni / ZrO2 catalyst: adding Ni / ZrO2 to 30 ml of dichloromethane and 5 mmol of C 17 H 38Si, after slowly stirring the solution evenly, add B(C6F5)3, continuously introduce hydrogen gas during the reaction process. After reacting for 20 minutes, rinse the sample with dichloromethane and hexane to wash away the residual and physically adsorbed hydrosilane. Then dry the sample again in a vacuum oven to obtain the emulsion Ni / ZrO2 catalyst. Given that it is difficult to distinguish the quality of the prepared emulsion Ni / ZrO2 catalyst with the naked eye, in this example, the emulsion Ni / ZrO2 catalyst is further used in the catalytic hydrogenation reaction of octanoic acid (process of the catalytic hydrogenation reaction of octanoic acid: ultrasonically disperse 0.1 g of the emulsion Ni / ZrO2 catalyst and 3 g of octanoic acid into a mixed solvent of 7.5 mL of deionized water and 42.5 mL of n-decane. Transfer the system to a 100 mL stainless steel autoclave reactor. The reactor is purged with H2 three times to discharge impurity gases, and then pressurized with H2 to 2 MPa. The stirring rate is constant (200 rpm). Then heat the reactor to the required reaction temperature and maintain it for 2 h. After the reaction is completed, wait for the autoclave to cool to room temperature, take out the liquid sample, and use an Agilent GC6820 gas chromatograph to analyze the conversion rate of phenol and the yield of the reaction product). Finally, the quality of the emulsion Ni / ZrO2 catalyst is measured by the conversion rate of octanoic acid. Using the emulsifying catalyst reactor device provided in this example and the above 3 gas inlet methods, the conversion rates of octanoic acid of the three batches of emulsion Ni / ZrO2 catalysts prepared in the catalytic hydrogenation reaction of octanoic acid are as Figure 3 shown (repeated 3 times for each batch and taking the average value). It is not difficult to see that the gas inlet method has a certain effect on the emulsification reaction, and the gas inlet method B of the lower stirring shaft 3 has obvious advantages.

[0026] Similarly, in order to further discuss the role of the copper mesh 6, this example sets copper meshes of different specifications (50 / 100 / 150 / 200 meshes), and uses the device without a copper mesh as a comparative example. The conversion rates of octanoic acid of the five batches of emulsion Ni / ZrO2 catalysts prepared by the devices without a copper mesh and with 4 specifications of copper meshes (the catalyst preparation process is the same as described above) in the catalytic hydrogenation reaction of octanoic acid (the process of the catalytic hydrogenation reaction of octanoic acid is the same as described above) are as Figure 4 shown (repeated 3 times for each batch and taking the average value). It is not difficult to see that the setting of the copper mesh 6 is indeed beneficial to the performance of the emulsifying catalyst, and the 100-mesh copper mesh has obvious advantages.

[0027] The above embodiments are only one of the preferred embodiments of the present invention and should not be used to limit the protection scope of the present invention. Any modification or polishing made without substantial meaning in the main design concept and spirit of the present invention, as long as the technical problems solved are still the same as those of the present invention, should be included in the protection scope of the present invention.

Claims

1. An emulsified catalyst reactor device, comprising a reaction vessel and a stirring device, characterized in that: The stirring device is composed of an upper stirring device and a lower stirring device which are independently arranged up and down and rotate in opposite directions. The upper stirring device and the lower stirring device are separated by a partition net.

2. The emulsified catalyst reactor device according to claim 1, characterized in that: The separation net is a copper net.

3. The emulsified catalyst reactor device according to claim 2, characterized in that: The specification of the copper mesh is 50-150 meshes.

4. The emulsified catalyst reactor device according to claim 3, characterized in that: The specification of the copper mesh is 100 meshes.

5. The emulsified catalyst reactor device according to claim 1, characterized in that: The rotating shaft of at least one of the upper stirring device and the lower stirring device is configured as a hollow shaft for ventilation.

6. The emulsified catalyst reactor device according to claim 5, characterized in that: The rotating shaft of the lower stirring device among the upper stirring device and the lower stirring device is configured as a hollow shaft for ventilation.

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