CN212410532U - Anthraquinone hydrogenation catalyst evaluation device - Google Patents
Anthraquinone hydrogenation catalyst evaluation device Download PDFInfo
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- CN212410532U CN212410532U CN202020982452.5U CN202020982452U CN212410532U CN 212410532 U CN212410532 U CN 212410532U CN 202020982452 U CN202020982452 U CN 202020982452U CN 212410532 U CN212410532 U CN 212410532U
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Abstract
The utility model discloses an anthraquinone hydrogenation catalyst evaluation device, press from both sides cover, back flow including packing inner tube, heat preservation, the inner tube that packs loads anthraquinone hydrogenation catalyst and inert filler, packs inner tube bottom and is network structure. The two ends of the return pipe are respectively connected with the upper end and the lower end of the packing inner pipe, a gas flowmeter is mounted at the front end of the inlet of the gas guide pipe, the outlet end of the return pipe penetrates through the lower end of the packing inner pipe and is slightly arranged in the pipe orifice at the inlet of the lower end of the return pipe, hydrogen is metered by the gas flowmeter and mixed with working liquid to pass through the outlet at the upper end of the return pipe, the hydrogen passes through the packing layer from top to bottom, the gas guide pipe and the packing inner pipe are arranged in a U. The evaluation device has the advantages of simple structure, easy operation and good evaluation data repeatability, and can effectively reflect the performance of the catalyst.
Description
Technical Field
The utility model relates to an anthraquinone hydrogenation catalyst evaluation device, the specially adapted anthraquinone hydrogenation prepares palladium catalyst evaluation device for hydrogen peroxide solution.
Background
The anthraquinone hydrogenation process is the most critical link in the production of hydrogen peroxide by an anthraquinone process, wherein an alumina catalyst is the most main catalyst in the prior anthraquinone hydrogenation process. The device for evaluating the alumina catalyst in the laboratory is key equipment which is necessary to be used in the research, development, production and use processes of the catalyst, and has the main functions of: the hydrogenation performance, the anthraquinone conversion efficiency and the anthraquinone degradation content of the palladium catalyst are quickly, accurately and simply evaluated.
Chinese patent (application No. CN201420800663) discloses a miniature evaluation device for anthraquinone hydrogenation catalysts, which comprises a high-pressure reaction kettle, magnetons, a heating coil and a catalyst frame, wherein the high-pressure reaction kettle is a sealed cylindrical container. This evaluation device catalyst frame sets up in high-pressure batch autoclave, because hydrogen is by the high-speed rotatory homodisperse of magneton, has improved the dissolution and the diffusion of hydrogen, has also led to partial hydrogen to fill the region between high-pressure batch autoclave and the catalyst frame easily for partial raw materials have no way to react, has also wasted partial hydrogen, thereby makes monitoring data unstable, the repeatability is poor, and the evaluation efficiency is low moreover.
Chinese patent CN 208003919U discloses an evaluation device for anthraquinone hydrogenation catalyst, which comprises a filler column, a heat-preservation jacket and a return pipe, wherein the heat-preservation jacket is wrapped on the outer wall of the filler column, the two ends of the return pipe are respectively connected with an inlet pipe and an outlet pipe of the filler column, and a gas conduit is designed at the bottom of the outlet pipe. In order to prevent that partial hydrogen from getting into to the back flow, this application is connected to different positions with gas conduit's gas outlet and back flow one end mouth of pipe, and up through the packing layer is followed to hydrogen, and gas-liquid mixture is poor, and the working solution backward flow effect is poor, and hydrogen flow also uncontrollable simultaneously, the buffer bottle of gas outlet is poor to the recovery effect of working solution to lead to reaction result unstability, repeatability poor. And when the ventilation is stopped, the working liquid can reversely flow into the gas conduit to cause pollution.
At present, the anthraquinone hydrogenation process is generally adopted in the industrial hydrogen peroxide production, and a palladium catalyst is the core of the process production. The performance of the catalyst directly determines the operational efficiency of the device. Therefore, the novel anthraquinone hydrogenation catalyst evaluation device has good guiding value for experimental research and product performance inspection.
SUMMERY OF THE UTILITY MODEL
In order to solve the defects of the prior art, the utility model aims at providing an anthraquinone hydrogenation catalyst evaluation device, which has the characteristics of simple structure, easy operation, good repeatability of evaluation results and the like, and ensures that the evaluation data can effectively react the catalyst performance.
In order to realize the purpose, the technical scheme of the utility model is that:
an anthraquinone hydrogenation catalyst evaluation device comprises a filler inner tube 3, a heat preservation jacket 2, a return tube 7 and a gas conduit 5, wherein the filler inner tube 3 is filled with an anthraquinone hydrogenation catalyst and inert fillers, and the bottom of the filler inner tube 3 is of a net structure; the two ends of the return pipe 7 are respectively connected with the upper end and the lower end of the filler inner pipe 3, the outlet end of the gas conduit 5 penetrates through the lower end of the filler inner pipe 3 and is slightly arranged in a pipe orifice at the inlet at the lower end of the return pipe 7, and after the hydrogen and the working fluid are mixed and pass through the upper port of the return pipe 7, the hydrogen and the working fluid pass through a filler layer jointly composed of the anthraquinone hydrogenation catalyst and the inert filler from top to bottom to form gas-liquid circulation of the working fluid; the gas conduit 5 and the inner filler pipe 3 are arranged in a U-shaped tubular shape; the heat-insulating jacket 2 is wrapped on the outer wall of the filler inner pipe 3.
Preferably, the device also comprises a reflux condensation pipe 1, wherein one end of the reflux condensation pipe 1 is connected with the outlet end of the packing inner pipe 3, and the other end of the reflux condensation pipe is a gas emptying outlet.
Preferably, the circulating cooling device further comprises a circulating cooling device, the reflux condensation pipe 1 is provided with an inlet and an outlet for circulating a cooling medium, and the circulating cooling device realizes the circulation of the cooled medium through the inlet and the outlet of the reflux condensation pipe 1.
Preferably, a gas flow meter 4 is included, said gas flow meter 4 being arranged at the front end of the inlet of said gas conduit 5.
Preferably, a first inert filler layer, an anthraquinone hydrogenation catalyst layer and a second inert filler layer are sequentially arranged from one end of the filler inner tube to the other end of the filler inner tube.
Preferably, the filler in the first inert filler layer and the second inert filler layer is glass balls with the diameter of 2-3 mm.
Preferably, the heat-insulation device also comprises a circulating constant temperature device 6, wherein the heat-insulation jacket 1 is provided with an inlet and an outlet, and the circulating constant temperature device is also provided with an inlet and an outlet which are respectively connected with the outlet and the inlet of the heat-insulation jacket 1.
Preferably, the lower end of the inner packing tube 3 is provided with a sampling port and a sampling valve 8.
Preferably, the material of the anthraquinone hydrogenation catalyst evaluation device is glass.
The utility model has the advantages that:
1. the feed gas is used as a power source, and the inlet is slightly arranged in the pipe orifice at the inlet at the lower end of the return pipe, so that the automatic circulation and return of the working liquid can be realized, and the gas-liquid mixing effect is good.
2. The gas flowmeter is designed at the inlet of the gas conduit, and the gas flow can be accurately controlled.
3. The constant-temperature circulating hot water is used as a heating medium and is directly heated by the jacket, the temperature is controlled to be +/-0.1 ℃, and the temperature control precision is high.
4. The outlet of the inner tube of the filler is provided with a reflux condenser tube, so that the working liquid carried by the airflow passing through the filler and the liquid layer can be effectively recovered.
5. The evaluation device is made of glass materials, and the reaction condition of the bed layer can be visually observed.
6. The evaluation device is simple to operate, stable in data and good in repeatability.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, are included to provide a further understanding of the application, and the description of the illustrative embodiments of the application and the description of the disclosure are intended to be illustrative of the application and are not intended to limit the application.
FIG. 1 is a schematic view of the structure of an evaluation apparatus in example 1.
Fig. 2 is an enlarged view of a portion of the bottom of the device shown in fig. 1.
The system comprises a reflux condenser pipe 1, a heat-preservation jacket 2, a packing inner pipe 3, a gas flowmeter 4, a gas guide pipe 5, a gas guide pipe 6, a circulating constant temperature device 7, a reflux pipe 8, a sampling valve 31, a first inert packing layer 32, an anthraquinone hydrogenation catalyst layer 33 and a second inert packing layer.
Detailed Description
It should be noted that the following detailed description is exemplary and is intended to provide further explanation of the disclosure. 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 application belongs.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of example embodiments according to the present application. As used herein, the singular forms "a", "an" and "the" are intended to include the plural forms as well, and it should be understood that when the terms "comprises" and/or "comprising" are used in this specification, they specify the presence of stated features, steps, operations, devices, components, and/or combinations thereof, unless the context clearly indicates otherwise.
As introduced in the background art, the prior art has the defects of unstable detection data and poor repeatability, and in order to solve the technical problems, the application provides an anthraquinone hydrogenation catalyst evaluation device.
The application provides a typical embodiment, provides an anthraquinone hydrogenation catalyst evaluation device, including filler inner tube, heat preservation jacket, back flow, the anthraquinone hydrogenation catalyst and inert filler are filled to the filler inner tube, and filler inner tube bottom is network structure. The two ends of the return pipe are respectively connected with the upper end and the lower end of the inner packing pipe, the front end of the inlet of the gas guide pipe is provided with a gas flowmeter, the outlet end of the gas guide pipe penetrates through the lower end of the inner packing pipe and is slightly arranged in a pipe orifice at the inlet of the lower end of the return pipe (for example, the outer diameter of the gas guide pipe is slightly smaller than the inner diameter of the return pipe, the gas guide pipe penetrates through the inner packing pipe and is inserted into the return pipe, the insertion degree of the gas guide pipe is very small), the gas guide pipe and the inner packing pipe are arranged in a U-shaped pipe shape, hydrogen passes through the upper end.
This application uses hydrogen to realize automatic backward flow circulation as the power supply messenger working solution between packing inner tube and back flow, places the exit end of gas conduit in the pipe orifice of back flow lower extreme entrance slightly in, and hydrogen and working solution mix through the back flow on the port after, from last down through the packing layer, form working solution gas-liquid circulation, and gas-liquid mixture is effectual, and the working solution circulation backward flow is effectual. The gas flowmeter is arranged at the front end of the gas conduit, so that the gas flow can be accurately controlled, the reflux rate of the working fluid is further controlled, the detection data are more stable, and the repeatability of the detection data is improved.
In order to prevent the gas from entraining the working fluid, it is preferable to include a reflux condenser tube connected to the filler tube.
Further preferably, a circulation cooling device is included, and the cooling medium flows into the reflux condenser pipe.
In order to prevent the fluctuation of the gas flow rate, it is preferable to include a gas flow meter provided at the front end of the gas conduit
Preferably, a constant temperature heating device is included, and the heating medium flows into the heat-preserving jacket.
Preferably, one end of the filler inner tube to the other end sequentially comprises an inert filler layer, an anthraquinone hydrogenation catalyst layer and an inert filler layer.
Further preferably, the filler in the inert filler layer is glass balls with the diameter of 2-3 mm.
For convenience of sampling, the lower end of the inner filler pipe is preferably provided with a sampling port.
Preferably, the material is glass.
In order to make the technical solutions of the present application more clearly understood by those skilled in the art, the technical solutions of the present application will be described in detail below with reference to specific embodiments.
Example 1
An anthraquinone hydrogenation catalyst evaluation device is made of glass and has a structure shown in figure 1, and comprises a filler inner pipe, a heat preservation jacket and a return pipe. The packing comprises an inert packing layer, an anthraquinone hydrogenation catalyst layer and an inert packing layer from one end to the other end of the packing inner tube in sequence, wherein the packing in the packing layer is a glass ball with the diameter of 2-3 mm, the packing layer is 5cm, and the anthraquinone hydrogenation catalyst layer is 20 cm. Packing bottom of the tubes is network structure, packing inner tube upper end and lower extreme are connected respectively to the both ends of back flow, gas flowmeter is equipped with to gas conduit import front end, the exit end passes packing inner tube lower extreme and places the mouth of pipe of back flow lower extreme entrance in a little in, it is the U-shaped tubulose with the packing inner tube and arranges, gas conduit is the U-shaped pipe with the packing inner tube and arranges, the heat preservation presss from both sides the cover parcel on the packed column outer wall, rivers after the water bath heater heating are gone into to the heat preservation and is pressed from both sides the cover, the reflux condenser pipe is connected with the packing tube, the coolant.
The using method comprises the following steps:
1. and sequentially filling inert fillers and hydrogenation catalysts into the filler inner tube.
2. The anthraquinone hydrogenation catalyst evaluation device is vertically placed and fixed on an iron support.
3. 70mL of prepared anthraquinone working solution is added through the upper end of the inner tube of the filler.
4. And fixing the reflux condenser pipe at the upper end of the inner filler pipe, starting the circulating cooling equipment, and enabling the cooling liquid to flow into the reflux condenser pipe.
5. And starting a circulating water bath for heating, and enabling the heated water to flow into the heat-preservation jacket.
6. When the working liquid in the filler pipe reaches the required temperature, the gas flow is controlled by the gas flowmeter, the hydrogen enters the return pipe through the gas guide pipe, and the working liquid starts to circulate and return.
7. The reaction was stopped after 30min and the hydrogenation liquid was discharged through the bottom outlet of the packed tube. The catalyst hydrogenation efficiency was then calculated after pipette sampling and oxidative extraction.
The following table shows the catalyst evaluation results of an anthraquinone hydrogenation catalyst evaluation device of the present invention.
TABLE 1 catalyst evaluation results comparison Table
| 1# | 2# | 3# | |
| Volume of working solution/mL | 70 | 70 | 70 |
| Catalyst adsorption volume/mL | 15 | 15 | 15 |
| Volume of hydrogenation solution/mL | 51.5 | 52.0 | 51.5 |
| Hydrogenation efficiency/g/mL | 8.16 | 8.08 | 8.16 |
The catalyst evaluation result shows that the device has good stability and repeatability of the evaluation result.
The matter described in this specification is only an example of a form of implementation of the inventive concept and the scope of protection of the invention should not be seen as being limited to the specific form set forth in the examples.
Claims (10)
1. An anthraquinone hydrogenation catalyst evaluation device is characterized in that:
the device comprises a filler inner pipe, a heat-preservation jacket, a return pipe and a gas guide pipe, wherein the filler inner pipe is filled with an anthraquinone hydrogenation catalyst and an inert filler, and the bottom of the filler inner pipe is of a net structure;
the two ends of the return pipe are respectively connected with the upper end and the lower end of the inner filler pipe, and hydrogen and working fluid are mixed and pass through a filler layer jointly formed by the anthraquinone hydrogenation catalyst and the inert filler from top to bottom after passing through an outlet at the upper end of the return pipe, so that gas-liquid circulation of the working fluid is formed;
the outlet end of the gas conduit penetrates through the lower end of the inner packing tube and is slightly arranged in a tube orifice at the inlet of the lower end of the return tube, and the outlet end of the gas conduit and the inner packing tube are arranged in a U-shaped tubular shape;
the heat-insulating jacket is wrapped on the outer wall of the filler inner pipe.
2. The apparatus for evaluating an anthraquinone hydrogenation catalyst according to claim 1, wherein:
the device also comprises a reflux condenser pipe, wherein one end of the reflux condenser pipe is connected with the outlet end of the filler inner pipe, and the other end of the reflux condenser pipe is a gas emptying outlet.
3. The apparatus for evaluating an anthraquinone hydrogenation catalyst according to claim 2, wherein:
the circulating cooling device is characterized by further comprising circulating cooling equipment, the backflow condensation pipe is provided with an inlet and an outlet for cooling medium circulation, and the circulating cooling equipment realizes circulation of cooled medium through the inlet and the outlet of the backflow condensation pipe.
4. The apparatus for evaluating an anthraquinone hydrogenation catalyst according to claim 1, wherein:
comprises a gas flow meter arranged at the front end of the inlet of the gas conduit.
5. The apparatus for evaluating an anthraquinone hydrogenation catalyst according to claim 1, wherein:
and a first inert filler layer, an anthraquinone hydrogenation catalyst layer and a second inert filler layer are sequentially arranged from one end to the other end of the filler inner tube.
6. The apparatus for evaluating an anthraquinone hydrogenation catalyst according to claim 5, wherein:
the filler in the first inert filler layer and the second inert filler layer is glass balls with the diameter of 2-3 mm.
7. The apparatus for evaluating an anthraquinone hydrogenation catalyst according to any one of claims 1 to 6, wherein:
the heat-insulation jacket is provided with an inlet and an outlet, and the circulating constant temperature equipment is also provided with an inlet and an outlet which are respectively connected with the outlet and the inlet of the heat-insulation jacket.
8. The apparatus for evaluating an anthraquinone hydrogenation catalyst according to any one of claims 1 to 6, wherein:
the lower end of the filler inner pipe is provided with a sampling port and a sampling valve.
9. The apparatus for evaluating an anthraquinone hydrogenation catalyst according to claim 1, wherein:
the material of the anthraquinone hydrogenation catalyst evaluation device is glass.
10. The apparatus for evaluating an anthraquinone hydrogenation catalyst according to claim 5, wherein:
the thickness of the first inert filler layer and the second inert filler layer is 5cm, and the thickness of the anthraquinone hydrogenation catalyst layer is 20 cm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN202020982452.5U CN212410532U (en) | 2020-06-02 | 2020-06-02 | Anthraquinone hydrogenation catalyst evaluation device |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202020982452.5U CN212410532U (en) | 2020-06-02 | 2020-06-02 | Anthraquinone hydrogenation catalyst evaluation device |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114749111A (en) * | 2022-04-21 | 2022-07-15 | 云南电网有限责任公司电力科学研究院 | Reactor for testing hydrogen absorption and desorption performance of organic liquid hydrogen storage material |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114749111A (en) * | 2022-04-21 | 2022-07-15 | 云南电网有限责任公司电力科学研究院 | Reactor for testing hydrogen absorption and desorption performance of organic liquid hydrogen storage material |
| CN114749111B (en) * | 2022-04-21 | 2024-03-19 | 云南电网有限责任公司电力科学研究院 | Reactor for testing hydrogen absorption and desorption performance of organic liquid hydrogen storage material |
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