Platinum-carbon catalyst synthesis integrated device and method capable of automatically controlling oil bath heating temperature

Abstract

The invention discloses a platinum carbon catalyst synthesis integration device and method capable of automatically controlling oil bath heating temperature, the device comprises a slurry constant temperature storage tank, a conveying pipeline, a slurry non-contact variable frequency stepless speed regulation conveying pump, an oil bath heating device, a cooling device, a slurry storage tank and a computer, the slurry constant temperature storage tank is communicated with the conveying pipeline; the conveying pipeline is provided with a slurry non-contact variable-frequency stepless speed regulation conveying pump, and the conveying pipeline is communicated with a slurry storage tank after sequentially passing through an oil bath heating device and a cooling device. The characteristics of high boiling point and fast heat conduction of edible rapeseed oil or peanut oil are utilized to heat the slurry of the platinum-carbon catalyst as an oil bath heat energy carrier, so that the internal chemical reaction is promoted, and the synthesis of the platinum-carbon catalyst is realized; and heating, cooling, and accurate control of temperature and flow velocity are integrated into one system, so that large-batch and automatic synthesis of the platinum-carbon catalyst is realized.

Description

Technical Field

[0001] The invention relates to the technical field of hydrogen energy industry, and in particular to an integrated device and method for synthesizing a platinum-carbon catalyst with automatic control of oil bath heating temperature. Background Art

[0002] Develop the hydrogen energy industry, utilize renewable energy sources such as wind, light, and tides to produce hydrogen, use hydrogen as an energy carrier, enable long-distance pipeline transportation, and then use hydrogen to generate electricity.

[0003] Whether it is PEM electrolysis of water to produce hydrogen, or proton exchange membrane fuel cells using hydrogen to generate electricity, catalysts prepared from "platinum group metals" are required. Among them, the most mature "platinum-carbon catalyst" has been widely used.

[0004] The membrane electrode in the PEM electrolyzer is coated with a platinum-carbon catalyst. Under the action of electric current, the platinum (Pt) atoms absorb the hydrogen (H) atoms in the water molecules, decomposing them into hydrogen and oxygen, and emitting hydrogen (H2) and oxygen (O2).

[0005] There is also a membrane electrode in hydrogen fuel cells, which consists of an anode, a cathode and a proton exchange membrane. The anode is where the hydrogen fuel is oxidized, and the cathode is where the oxidant is reduced. Both electrodes contain platinum-carbon catalysts that accelerate the electrochemical reaction of the electrodes. Platinum (Pt) is used as a catalyst material. After hydrogen molecules are adsorbed on the surface of platinum, the molecules are split into atomic states at the adsorption point, and a reaction occurs at low temperatures, thereby generating current and discharging water at the same time. No harmful substances are discharged.

[0006] It can be seen that platinum-carbon catalysts play a vital role in both PEM electrolysis of water to produce hydrogen and hydrogen fuel cells using hydrogen to generate electricity, and are directly related to the performance, life and cost of PEM electrolyzers and fuel cells.

[0007] At present, small batch preparation generally adopts the method of placing a magnetic stirrer in a beaker for heating synthesis. The manual operation is very cumbersome, the degree of automation is not high, and the output is extremely low, which seriously restricts the development of fuel cell catalyst production. At present, the domestic procurement of platinum-carbon catalysts mainly relies on foreign imports.

[0008] Therefore, there is a huge market space for the research and development of large-scale platinum-carbon catalyst production facilities and equipment. Summary of the invention

[0009] The purpose of the present invention is to provide an integrated device and method for synthesizing a platinum-carbon catalyst with automatic control of the oil bath heating temperature, so as to solve the current problems of difficulty in synthesizing the platinum-carbon catalyst and low yield.

[0010] To achieve the above-mentioned purpose, the present invention provides the following technical scheme: an integrated device for synthesizing platinum-carbon catalysts with automatic control of oil bath heating temperature, comprising a slurry constant temperature storage tank, a delivery pipeline, a slurry non-contact variable frequency stepless speed regulation delivery pump, an oil bath heating device, a cooling device, a slurry storage tank and a computer, the slurry constant temperature storage tank is connected to the delivery pipeline, the slurry non-contact variable frequency stepless speed regulation delivery pump is arranged on the delivery pipeline, the delivery pipeline is connected to the slurry storage tank after passing through the oil bath heating device and the cooling device in sequence; an oil temperature monitor is arranged in the oil bath heating device, a water temperature monitor is arranged in the cooling device, the oil temperature monitor and the water temperature monitor are respectively connected to the computer, the monitoring data of the oil temperature monitor corresponds to the temperature control of the oil bath heating device, and the monitoring data of the water temperature monitor corresponds to the temperature control of the cooling device.

[0011] Preferably, the slurry constant temperature storage tank comprises two layers, an inner layer being a slurry storage space and an outer layer being circulating constant temperature water.

[0012] Preferably, the oil bath heating device comprises an oil tank filled with rapeseed oil or peanut oil, wherein a heating tube, an oil stirrer and an oil bath coil support are arranged in the oil tank.

[0013] Preferably, the oil bath coil support comprises a plurality of vertical plates distributed in a cylindrical shape, and inner and outer sides of the vertical plates are respectively provided with slots for inserting into the conveying pipeline.

[0014] Preferably, the oil tank is provided with a cotton protective cover.

[0015] Preferably, a non-contact flow monitor and a non-contact temperature monitor, which are respectively connected to a computer, are provided at the slurry outlet of the oil bath heating device.

[0016] Preferably, the cooling device comprises a cooling water tank, in which a cooling water agitator and a cooling coil bracket are arranged.

[0017] Preferably, the cooling water tank is cyclically connected to the cooling water tower via a pipeline.

[0018] Preferably, a non-contact flow monitor 2 and a non-contact temperature monitor 2, which are respectively connected to a computer, are provided at the slurry outlet of the cooling device.

[0019] The present invention also provides a method for synthesizing a platinum-carbon catalyst with automatic oil bath heating temperature control, comprising the following steps:

[0020] Step 1: First, pour the prepared catalyst slurry into a slurry constant temperature storage tank;

[0021] Step 2: Start the computer, run the process program of the catalyst product to be produced, and control the oil temperature of the oil bath heating device and the water temperature of the cooling device to reach the predetermined parameters;

[0022] Step 3: The non-contact variable frequency stepless speed regulating delivery pump starts to work, so that the catalyst slurry enters the oil bath heating device along the delivery pipeline, and the catalyst slurry is heated to 160° C. to 180° C. in the oil bath heating device and maintained for 30s to 50s;

[0023] Step 4: After the catalyst slurry completes the reaction in the oil bath heating device, it flows along the conveying pipeline through the cooling device to be cooled to 50°C to 60°C, and finally flows into the slurry storage tank.

[0024] Compared with the prior art, the present invention has the following beneficial effects: the present invention utilizes the high boiling point and fast heat conduction characteristics of edible rapeseed oil or peanut oil to serve as an oil bath heat energy carrier to heat the slurry of the platinum-carbon catalyst, promote chemical reactions inside the slurry, and realize the synthesis of the platinum-carbon catalyst; and integrates the precise control of heating, cooling, temperature and flow rate into one system to realize the large-scale, automated synthesis of the platinum-carbon catalyst. BRIEF DESCRIPTION OF THE DRAWINGS

[0025] Figure 1 It is a schematic diagram of the overall structure of the present invention.

[0026] Figure 2 It is a structural schematic diagram of the oil bath heating device in the present invention.

[0027] Figure 3 It is a schematic diagram of the structure of the cooling device in the present invention.

[0028] Figure 4 It is a curve diagram of catalyst slurry temperature control in the present invention.

[0029] Figure 5 It is a schematic diagram of the coil support structure in the present invention. DETAILED DESCRIPTION

[0030] In order to make the purpose, technical solutions and advantages of the present invention more clearly understood, the present invention is further specifically described below through embodiments.

[0031] Example: An integrated device for synthesizing platinum-carbon catalyst with automatic control of oil bath heating temperature, referring to Figure 1-5 , including a slurry constant temperature storage tank 1, a conveying pipeline 2, a slurry non-contact variable frequency stepless speed regulation conveying pump 3, an oil bath heating device 4, a cooling device 5, a non-contact temperature monitor 7, a non-contact flow monitor 6, a cooling water tower 11, a water pump 8, a flow monitor 9, a temperature monitor 10, a non-contact temperature monitor 2 15, a non-contact flow monitor 2 14, a slurry storage tank 13 and a control center computer 12.

[0032] The slurry constant temperature storage tank 1 is connected to the delivery pipeline 2, and the slurry non-contact variable frequency stepless speed regulation delivery pump 3 is arranged on the delivery pipeline 2. The delivery pipeline 2 is connected to the slurry storage tank after passing through the oil bath heating device 4 and the cooling device 5 in sequence.

[0033] The slurry non-contact variable frequency stepless speed regulation delivery pump 3, oil bath heating device 4, cooling device 5, non-contact temperature monitor 7, non-contact flow monitor 6, water pump 8, flow monitor 9, temperature monitor 10, cooling water tower 11, non-contact temperature monitor 15, non-contact flow monitor 14 are connected to the computer. The computer controls the speed of the variable frequency stepless speed regulation delivery pump 3 and the temperature of the edible rapeseed oil 4c (or peanut oil) in the oil bath heating device 4 through feedback and analysis of temperature and flow data, and controls the cooling device 5 to realize automated production and record the process parameters of the entire production process.

[0034] The slurry constant temperature storage tank 1 is divided into two layers, the inner layer is the slurry storage space 1a, and the outer layer is the circulating constant temperature water 1b, to ensure that the temperature of the slurry entering the oil bath heating device 4 is relatively constant. The slurry in the slurry constant temperature storage tank 1 is transported by the slurry non-contact variable frequency stepless speed regulation delivery pump 3.

[0035] The oil bath heating device 4 is composed of an oil tank 4b containing edible rapeseed oil 4c (or peanut oil), a cotton protective cover 4d covering the outside of the oil tank 4b, a heating tube 4e for heating, an oil temperature monitor 4m for monitoring the oil temperature, an oil agitator 4a, an oil bath coil bracket 4h, and a stirring wheel 4f installed on the oil agitator 4a.

[0036] Edible rapeseed oil 4c (or peanut oil) has the highest boiling point among edible oils, reaching 335°C, and has high thermal conductivity. Our slurry heating temperature is around 180°C, so rapeseed oil 4c (or peanut oil) is the best choice.

[0037] The oil bath coil support 4h is composed of four vertical plates 4h1, four horizontal plates 4h2, and four cross-fork fixing plates 4h3, which are connected together by bolts 4h4 to form a quasi-cylindrical frame. There are slots 4h5 on the inner and outer sides of the vertical plate 4h1, and a notch 4h6 with a diameter slightly smaller than the hole 4h5 is opened on the outer side of the slot 4h5. The conveying pipeline is inserted into the slot 4h5 through the notch 4h6, which is convenient and quick to install. The conveying pipeline is attached to the oil bath coil support 4h in two layers, inner and outer, and the whole is immersed in edible rapeseed oil 4c (or peanut oil) to fully ensure that the slurry is heated and completes the chemical reaction.

[0038] The oil bath heating device 4 is provided with a non-contact flow monitor 6 and a non-contact temperature monitor 7 at its slurry outlet, both of which are connected to a computer 12. The computer is responsible for analyzing the collected flow rate and temperature and issuing instructions.

[0039] The oil temperature monitor 4m is connected to the computer 12 via a data line, and the computer 12 collects and analyzes the temperature of the edible rapeseed oil 4c (or peanut oil) in real time.

[0040] The computer 12 analyzes the collected edible rapeseed oil 4c (or peanut oil) temperature, slurry flow parameters, and slurry temperature parameters, and then sends instructions to the slurry non-contact variable frequency stepless speed regulation delivery pump 3 and heating tube 4e to adjust the speed of the delivery pump 3 and the heating power parameters of the heating tube 4e to ensure that the slurry flowing through the oil bath heating device 4 completes the chemical reaction at the optimal temperature and optimal reaction time.

[0041] The cooling device 5 is composed of a cooling water tank 5c, cooling water 5d, a water temperature monitor 5b, a cooling water stirrer 5a, stirring blades 5g installed on the cooling water stirrer 5a, and a cooling water coil bracket 5e.

[0042] The cooling water coil support 5e has the same structure as the oil bath coil support 4h. The same delivery pipeline 2 is divided into two layers, inner and outer, and is attached to the cooling water pipe support 5e and is immersed in the cooling water 5d as a whole.

[0043] The cooling water tank 5c is cyclically connected to the cooling water tower 11 through a pipeline, and a water pump 8 is provided on the pipeline. The cooling water 5d circulates between the cooling water tower 11 and the cooling water tank 5c by the water pump, and the low-temperature water enters the cooling water tank 5c, absorbs the heat of the slurry and heats up to become high-temperature water, and the high-temperature water returns to the cooling tower 11, and the cooling tower 11 dissipates the heat of the high-temperature water and becomes low-temperature cooling water 5d.

[0044] The water temperature monitor 5b installed in the cooling water tank 5c is connected to the computer 12 via a data line. The computer 12 collects temperature data in real time as a basis for issuing instructions to the water pump 8 and the cooling water tower 11.

[0045] The slurry outlet of the cooling device 5 is provided with a non-contact flow monitor 2 14 and a non-contact temperature monitor 2 15, both of which are connected to the computer 12. The computer 12 is responsible for analyzing the collected flow rate and temperature as the basis for issuing instructions to the water pump 8 and the water temperature control of the cooling water tower 9. At the same time, the computer 12 makes a judgment on production failure, shutdown alarm, and shutdown and issues instructions by comparing the parameters of the non-contact flow monitor 2 14 and the non-contact flow monitor 2 6.

[0046] After being cooled, the catalyst slurry finally enters the slurry storage tank 13 to be transferred to the subsequent process.

[0047] The pipe connecting the cooling water tank 5c and the cooling water tower 11 is provided with a temperature tester 10 and a flow monitor 9, which are connected to a computer 12 via a data line. The computer 12 analyzes and calculates the captured temperature and flow, and then sends instructions to the cooling water tower 11 and the water pump 8 to adjust the water temperature and circulation flow entering the cooling water tank 5c, so that the temperature of the catalyst slurry drops below the required temperature within a specified time.

[0048] This embodiment, when implemented, includes the following steps:

[0049] Step 1: First, pour the prepared catalyst slurry into the slurry constant temperature storage tank 1. The slurry constant temperature storage tank 1 is divided into two layers, the inner layer is the slurry storage space 1a, and the outer layer is the circulating constant temperature water storage space 1b. The constant temperature water is adjusted to 70℃~80℃ through an external constant temperature control device, and circulates in and out of the constant temperature water storage space 1b, so as to ensure that the catalyst slurry is always kept at 70℃~80℃.

[0050] Step 2: Start the computer 12 and run the process program of the catalyst product to be produced. This requires manual selection of the relevant program.

[0051] The oil agitator 4a and the cooling water agitator 5g are started to stir the rapeseed oil 4c (or peanut oil) and the cooling water 5d. The computer 12 captures the monitored temperature parameters of the rapeseed oil 4c (or peanut oil) and the cooling water 5d through the temperature monitor 4m and the temperature monitor 5b.

[0052] The heating function of the heating tube 4e is started to heat the rapeseed oil 4c (or peanut oil). When the temperature of the rapeseed oil 4c (or peanut oil) is higher than 200°C, the heating is stopped; when the temperature of the rapeseed oil 4c (or peanut oil) is lower than 180°C, the heating is resumed.

[0053] The water pump 8 is started to inject cooling water 5d into the cooling water tank 5c, and the cooling water 5d flows back to the cooling water tower 11 through the pipeline. The cooling water tower 11 sends a working instruction to the computer 12 based on the data fed back by the temperature monitor 10 (required not to be higher than 40°C): if the water temperature is higher than 40°C, the computer 12 sends an instruction to the cooling tower 11 to dissipate heat and cool the cooling water 5d until the temperature is lower than 40°C and stops working.

[0054] Step 3: The computer 12 sends a command to the non-contact variable frequency stepless speed regulating pump 3 to deliver the catalyst slurry to the oil bath heating device 4 at the speed specified by the program. When the catalyst slurry flows through the oil bath heating device 4, it is heated to about 170°C and maintained at this temperature for 30s to 50s. The substances in the catalyst slurry undergo a chemical reaction: platinum atoms are adsorbed on carbon atoms to form a platinum-carbon complex substance.

[0055] After the slurry after the reaction flows out of the oil bath heating device 4, the computer 12 captures the flow and temperature parameters through the non-contact flow monitor 6 and non-contact temperature monitor 7 attached to the delivery pipe 2, and compares them with the specified setting parameters to determine whether the reaction temperature and reaction time meet the requirements. Otherwise, an alarm is issued, and the speed of the slurry non-contact variable frequency stepless speed regulation delivery pump 3 is adjusted at the same time. It is ensured that when the catalyst slurry passes through the oil bath heating device 4, the reaction temperature and reaction time meet the requirements.

[0056] There are regulated requirements for the temperature and reaction time of the chemical reaction inside the catalyst slurry: the temperature is 160℃~180℃, and the reaction time is 30 seconds~50 seconds at this temperature.

[0057] The part of the delivery pipeline 2 that flows through the oil bath heating device 4 and the cooling device 5 is made of glass or tetrafluoroethylene, which has high acid resistance, alkali resistance and corrosion resistance.

[0058] Step 4: After the catalyst slurry completes the reaction in the oil bath heating device 4, it flows into the cooling device 5 through the delivery pipe 2. When the catalyst slurry in a high-heat state flows through the cooling device 5, it is cooled to about 50°C (the qualified range is below 60°C). This temperature will be monitored by the non-contact temperature monitor 15 set at the outlet of the cooling device 5, and the data will be transmitted to the computer 12. If the temperature value captured by the computer 12 is higher than 50°C, it will issue an instruction to adjust the flow rate of the water pump 8 and the outlet water temperature parameters of the cooling water tower 11. If the temperature value captured by the computer 12 is higher than 60°C, an alarm will be issued to prompt the staff to intervene in the equipment to solve the fault.

[0059] The catalyst material cooled to a specified temperature (50°C to 60°C) flows into the storage tank 13, and then enters the next "filtration and cleaning" process to obtain a wet catalyst product.

[0060] Step 5: Shutdown. When the feedback data of the flow meter 6 and the flow monitor 14 are both zero, the computer 12 will issue an alarm to prompt the personnel to intervene and shut down. If there is no personnel intervention within three minutes, the computer 12 will issue a command to shut down the machine to protect the equipment itself.

[0061] The cooling water tower 11 is responsible for dissipating heat and cooling the cooling water 5d. The water pump 8 is responsible for transporting the cooling water 5d from the cooling water tower 11 to the cooling water tank 5c, and the cooling water 5d flows back to the cooling water tower 11 through the reflux pipe. The flow monitor 9 and the temperature monitor 10 are responsible for monitoring the flow and temperature of the cooling water 5d flowing to the cooling water tank 5c. The computer 12 adjusts the heat dissipation intensity of the cooling water tower 11 and the speed of the water pump 8 by combining the captured flow and temperature data with the temperature parameters fed back by the temperature monitor 15. Ensure that the cooling function of the cooling device 5 is sufficient to cool the high-temperature catalyst slurry to the specified temperature of 50°C to 60°C.

[0062] The computer 12 will record the captured parameters with time as the ordinate and display them in the form of a graph curve, so that the operator can make an intuitive judgment.

[0063] The computer 12 will store the captured parameters in a time sequence in the form of a data table for later review and tracing.

[0064] The above embodiments are only for illustrating the technical concept and features of the present invention, and their purpose is to enable people familiar with the technology to understand the content of the present invention and implement it accordingly, and they cannot be used to limit the protection scope of the present invention. Any equivalent changes or modifications made according to the spirit of the present invention should be included in the protection scope of the present invention.

Claims

1. An integrated device for synthesizing platinum-carbon catalysts with automatic oil bath heating temperature control, characterized in that: It includes a slurry constant temperature storage tank, a delivery pipeline, a slurry non-contact variable frequency stepless speed regulation delivery pump, an oil bath heating device, a cooling device, a slurry storage tank and a computer. The slurry constant temperature storage tank is connected to the delivery pipeline, and the slurry non-contact variable frequency stepless speed regulation delivery pump is arranged on the delivery pipeline. The delivery pipeline is connected to the slurry storage tank after passing through the oil bath heating device and the cooling device in sequence. The oil bath heating device is provided with an oil temperature monitor, and the cooling device is provided with a water temperature monitor. The oil temperature monitor and the water temperature monitor are respectively connected to a computer, and the monitoring data of the oil temperature monitor is used for temperature control of the oil bath heating device, and the monitoring data of the water temperature monitor is used for temperature control of the cooling device.

2. The integrated device for synthesizing platinum-carbon catalyst with automatic control of oil bath heating temperature according to claim 1 is characterized in that: The slurry constant temperature storage tank comprises an inner and outer layer, wherein the inner layer is a slurry storage space and the outer layer is circulating constant temperature water.

3. The integrated device for synthesizing platinum-carbon catalyst with automatic control of oil bath heating temperature according to claim 1 is characterized in that: The oil bath heating device comprises an oil tank filled with rapeseed oil or peanut oil, wherein a heating pipe, an oil stirrer and an oil bath coil support are arranged in the oil tank.

4. The integrated device for synthesizing platinum-carbon catalyst with automatic control of oil bath heating temperature according to claim 3 is characterized in that: The oil bath coil support comprises a plurality of vertical plates distributed in a cylindrical shape, and the inner and outer sides of the vertical plates are respectively provided with slots for clamping into the conveying pipeline.

5. The integrated device for synthesizing platinum-carbon catalyst with automatic control of oil bath heating temperature according to claim 3 is characterized in that: A cotton protective cover is arranged outside the oil tank.

6. The integrated device for synthesizing platinum-carbon catalyst with automatic control of oil bath heating temperature according to claim 3 is characterized in that: A non-contact flow monitor 1 and a non-contact temperature monitor 1 which are respectively connected to a computer are provided at the slurry outlet of the oil bath heating device.

7. The integrated device for synthesizing platinum-carbon catalyst with automatic control of oil bath heating temperature according to claim 1, characterized in that: The cooling device comprises a cooling water tank, in which a cooling water agitator and a cooling coil bracket are arranged.

8. The integrated device for synthesizing platinum-carbon catalyst with automatic control of oil bath heating temperature according to claim 7, characterized in that: The cooling water tank is cyclically connected with the cooling water tower through a pipeline.

9. The integrated device for synthesizing platinum-carbon catalyst with automatic control of oil bath heating temperature according to claim 7, characterized in that: A second non-contact flow monitor and a second non-contact temperature monitor which are respectively connected to a computer are provided at the slurry outlet of the cooling device.

10. The synthesis method of the integrated device for synthesizing platinum-carbon catalyst with automatic oil bath heating temperature control as claimed in claim 1, characterized in that: The steps include: Step 1: First, pour the prepared catalyst slurry into a slurry constant temperature storage tank; Step 2: Start the computer, run the process program of the catalyst product to be produced, and control the oil temperature of the oil bath heating device and the water temperature of the cooling device to reach the predetermined parameters; Step 3: The non-contact variable frequency stepless speed regulating delivery pump starts to work, so that the catalyst slurry enters the oil bath heating device along the delivery pipeline, and the catalyst slurry is heated to 160° C. to 180° C. in the oil bath heating device and maintained for 30s to 50s; Step 4: After the catalyst slurry completes the reaction in the oil bath heating device, it flows along the conveying pipeline through the cooling device to be cooled to 50°C to 60°C, and finally flows into the slurry storage tank.

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