Palladium-carbon catalytic hydrogenation reaction material treatment system

Abstract

The invention relates to the technical field of chemical engineering, and particularly discloses a palladium-carbon catalytic hydrogenation reaction material treatment system, which comprises a three-dimensional workshop structure, an air-operated hoist, an air supply system, an air supply system and an air supply system, wherein the top of the three-dimensional workshop structure is provided with an elevator and a hoisting ton bag; the palladium-carbon circulating unit comprises a palladium-carbon preparation kettle, a hydrogenation reaction kettle, a decarbonization filter, a filter pressing cylinder, a sample splitter and a glove box which are connected in sequence, and the sample splitter is connected back to the palladium-carbon preparation kettle through a closed pipeline; the solid feeding unit comprises a ton bag feeder, a pneumatic valve and a spiral conveying pipe, and the tail end of the solid feeding unit is connected with a top feeding hole of the hydrogenation reaction kettle; the gas supply system comprises a hydrogen cylinder group and is connected to a gas distributor at the bottom of the hydrogenation reaction kettle through a pressure reducing valve and a flow regulating valve; through the multi-stage separation design and the safety interlocking mechanism of the palladium-carbon circulating unit, the recovery rate of the catalyst is increased, meanwhile, the pressure, temperature and stirring state are monitored in real time to trigger nitrogen purging or pressure relief, and the risks of hydrogen leakage and reaction out-of-control are reduced in combination with inert gas protection of the glove box.

Description

Technical Field

[0001] This patent belongs to the field of chemical technology, and specifically relates to a palladium-carbon catalytic hydrogenation reaction material processing system. Background Art

[0002] Palladium-carbon catalyzed hydrogenation reaction is a key technology widely used in organic synthesis, especially in the fields of medicine, pesticides and fine chemicals.

[0003] However, the existing palladium-carbon catalytic hydrogenation reaction material processing systems generally have the problem that the palladium-carbon catalyst is difficult to completely separate after the reaction, resulting in large catalyst losses and high costs. Some systems use simple filtration methods, but the filter element is easily clogged and the backflushing effect is poor.

[0004] Patent content

[0005] The purpose of this patent is to provide a palladium-carbon catalytic hydrogenation reaction material processing system to solve the problems raised in the above background technology.

[0006] To achieve the above purpose, this patent provides the following technical solutions:

[0007] A palladium-carbon catalytic hydrogenation reaction material processing system, comprising:

[0008] The three-dimensional workshop structure has a hoist and a pneumatic hoist for lifting ton bags on the top;

[0009] A palladium-carbon circulation unit comprises a palladium-carbon preparation kettle, a hydrogenation reaction kettle, a decarbonization filter, a filter press, a sample divider and a glove box which are connected in sequence, wherein the sample divider is connected back to the palladium-carbon preparation kettle through a closed pipeline;

[0010] A solid feeding unit, including a ton bag feeder, a pneumatic valve and a spiral conveying pipe, the end of which is connected to the feed port on the top of the hydrogenation reactor;

[0011] The gas supply system includes a hydrogen cylinder group connected to the gas distributor at the bottom of the hydrogenation reactor through a pressure reducing valve and a flow regulating valve;

[0012] The safety interlock system includes a pressure sensor, a temperature sensor and a stirring motor current monitor installed on the hydrogenation reactor, which are connected to the PLC controller to trigger the following actions:

[0013] a) When the pressure or temperature reaches the HH value, the hydrogen inlet valve is automatically closed and the nitrogen purge valve is opened;

[0014] b) When the stirring motor fails, the emergency pressure relief valve will be opened.

[0015] Preferably, a titanium metal sintered filter rod with a pore diameter of 0.5 - 5 μm is provided inside the decarbonization filter. An anti-blow nitrogen pipe is provided at the top of the filter, and the bottom is connected to a pressure filter cylinder through a pneumatic butterfly valve.

[0016] Preferably, the palladium-carbon preparation kettle is provided with a vacuum conveying pipeline, which is connected to the vacuum system of the hydrogenation reactor.

[0017] Preferably, the pressure filter cylinder comprises a structure in which multiple layers of filter cloth and filter plates are arranged alternately.

[0018] Preferably, a conical diversion structure is provided at the bottom of the hydrogenation reactor, the cone angle is 60°, and the inner wall polishing roughness Ra ≤ 0.4 μm.

[0019] Compared with the prior art, the beneficial effects of this patent are as follows:

[0020] (1) Through the multi-stage separation design and safety interlock mechanism of the palladium-carbon recycling unit, the catalyst recovery rate is improved. At the same time, the pressure, temperature and stirring state are monitored in real time to trigger nitrogen purging or pressure relief. Combined with the inert gas protection of the glove box, the risk of hydrogen leakage and reaction out of control is reduced.

[0021] (2) Through the PLC controller to link the feeding, gas supply and safety systems, full-process automatic control is realized. Description of the Drawings

[0022] Figure 1 is one of the three-dimensional drawings of this patent;

[0023] In the figure: 1. Palladium-carbon preparation kettle; 2. Hydrogenation reactor; 3. Decarbonization filter; 4. Pressure filter cylinder; 5. Sampler; 6. Glove box; 7. Tonneau bag feeder; 8. Hydrogen cylinder group. Detailed Embodiments

[0024] The technical solutions in the embodiments of this patent will be clearly and completely described below with reference to the drawings in the embodiments of this patent. Obviously, the described embodiments are only a part of the embodiments of this patent, rather than all the embodiments. All other embodiments obtained by those of ordinary skill in the art based on the embodiments in this patent without creative efforts shall fall within the protection scope of this patent.

[0025] Embodiment 1:

[0026] Please refer to Figure 1 as shown, a palladium-carbon catalytic hydrogenation reaction material processing system includes:

[0027] A three-dimensional workshop structure, with a hoist and a pneumatic hoist configured at the top of the workshop for lifting tonneau bag materials and positioning them to the tonneau bag feeder 7;

[0028] The pneumatic hoist uses compressed air as the power source to drive the motor to drive the internal mechanical components to meet the working requirements of lifting heavy objects. It will not generate any sparks during use, has explosion-proof function, high safety factor, high working efficiency, and the pressure is 0.4 - 0.6 MPa;

[0029] The palladium-carbon recycling unit includes a palladium-carbon preparation kettle 1, a hydrogenation reactor 2, a decarbonization filter 3, a pressure filter cylinder 4, a sampler 5 and a glove box 6 connected in sequence. Among them, the ratio of the sampled materials in the sample hopper of the sampler 5 is manually fed into the glove box and then into the solid materials according to the process ratio, and finally returns to the palladium-carbon preparation kettle 1 through a closed pipeline;

[0030] The glove box is for high-value powder closed feeding and conveying. When feeding powders with corrosiveness or toxicity, etc., it can protect the operator; it realizes the feeding and conveying of lightweight materials; it can be used for feeding explosion-proof materials or in explosion-proof environments, such as the feeding of materials like alumina; it is also used for feeding the reaction kettle; it can reduce solid dust, protect the on-site feeding environment, and reduce the risk of dust explosion;

[0031] The palladium-carbon preparation kettle 1 is connected to the hydrogenation reactor 2 through a vacuum conveying pipeline, and is internally equipped with a high-shear stirring device for uniformly mixing the palladium-carbon catalyst and the solvent;

[0032] The bottom of the hydrogenation reactor 2 is provided with a conical diversion structure with a cone angle of 60°, and the inner wall is polished with a roughness Ra ≤ 0.4 μm to ensure no residue of materials; the gas distributor is located at the bottom and is connected to the hydrogen cylinder group 8 through a pressure reducing valve and a flow regulating valve;

[0033] The decarbonization filter 3 is internally equipped with titanium metal sintered filter rods with a pore diameter of 0.5 - 5 μm, and an anti-blow nitrogen pipe is provided at the top for regularly cleaning the filter element; the bottom is connected to the pressure filter cylinder 4 through a pneumatic butterfly valve.

[0034] The pressure filter cylinder 4 adopts a structure of alternating multi-layer filter cloth and filter plates, and realizes efficient solid-liquid separation through hydraulic drive. The filtrate enters the downstream process, and the solid catalyst residue is recovered by the sampler 5.

[0035] The sampler 5 returns the recovered palladium-carbon catalyst to the palladium-carbon preparation kettle 1 through a closed pipeline to achieve recycling.

[0036] The glove box 6 is used for manually handling highly active materials or sampling catalysts under abnormal conditions to ensure operation safety;

[0037] The solid feeding unit includes a ton bag feeder 7, a pneumatic valve and a screw conveyor, and the end is connected to the top feed port of the hydrogenation reactor 2;

[0038] The ton bag feeder 7 controls the material flow rate through a pneumatic valve, and transports the solid raw materials to the top feed port of the hydrogenation reactor 2 through a screw conveyor, and the whole process is closed to avoid dust dispersion;

[0039] A gas supply system, including a hydrogen cylinder bank 8, which is connected to the gas distributor at the bottom of the hydrogenation reactor 2 through a pressure reducing valve and a flow regulating valve;

[0040] The hydrogen cylinder bank 8 adjusts the hydrogen pressure and flow through a two-stage pressure reducing valve and an electronic flowmeter to ensure a stable hydrogen concentration in the hydrogenation reactor 2;

[0041] A safety interlock system, including a pressure sensor, a temperature sensor and a stirrer motor current monitor provided on the hydrogenation reactor 2, which are respectively connected to a PLC controller;

[0042] The pressure sensor and the temperature sensor on the hydrogenation reactor 2 monitor the data in real time. When the pressure or temperature reaches the preset high-high (HH) value, the PLC controller automatically closes the hydrogen inlet valve and opens the nitrogen purge valve to quickly reduce the reaction activity;

[0043] If the stirrer motor current is abnormal, such as overload or stall, the PLC triggers the opening of the emergency pressure relief valve and stops the hydrogen supply at the same time to prevent the reaction from getting out of control.

[0044] As can be seen from the above, the bulk bag material is lifted to the feeder 7 by a pneumatic hoist and fed into the hydrogenation reactor 2 through a screw conveyor pipe. The catalyst slurry prepared in the palladium-carbon preparation kettle 1 is transported to the hydrogenation reactor 2 through a vacuum system. After starting the stirring and introducing hydrogen for catalytic hydrogenation reaction, after the reaction is completed, the material is preliminarily separated by a decarbonization filter 3, and the filtrate enters the pressure filter cylinder 4 for further fine filtration. The solid catalyst is recovered by a sampler 5 and recycled. In case of an abnormality, the safety interlock system automatically performs a nitrogen purge or pressure relief operation to ensure the safety of the system.

[0045] Although the embodiments of this patent have been shown and described, for those of ordinary skill in the art, it can be understood that various changes, modifications, substitutions and variations can be made to these embodiments without departing from the principle and spirit of this patent. The scope of this patent is defined by the appended claims and their equivalents.

Claims

1. A palladium-carbon catalytic hydrogenation reaction material processing system, characterized in that, include: The three-dimensional workshop structure has a hoist and a pneumatic hoist for lifting ton bags on the top; A palladium-carbon circulation unit comprises a palladium-carbon preparation kettle (1), a hydrogenation reaction kettle (2), a decarbonization filter (3), a filter press cylinder (4), a sample divider (5) and a glove box (6) which are connected in sequence, wherein the sample divider (5) is connected back to the palladium-carbon preparation kettle (1) through a closed pipeline; A solid feeding unit, comprising a ton bag feeder (7), a pneumatic valve and a spiral conveying pipe, the end of which is connected to the top feed port of the hydrogenation reactor (2); A gas supply system, comprising a hydrogen cylinder group (8), connected to a gas distributor at the bottom of the hydrogenation reactor (2) via a pressure reducing valve and a flow regulating valve; The safety interlock system includes a pressure sensor, a temperature sensor and a stirring motor current monitor arranged on the hydrogenation reactor (2), which are respectively connected to the PLC controller to trigger the following actions: a) When the pressure or temperature reaches the HH value, the hydrogen inlet valve is automatically closed and the nitrogen purge valve is opened; b) When the stirring motor fails, the emergency pressure relief valve will be opened.

2. The palladium-carbon catalytic hydrogenation reaction material processing system according to claim 1, wherein: The decarbonization filter (3) is provided with a titanium metal sintered filter rod with a pore size of 0.5-5 μm inside, a back-blowing nitrogen pipe is provided on the top of the filter, and the bottom is connected to the filter press cylinder (4) through a pneumatic butterfly valve.

3. A palladium-carbon catalytic hydrogenation reaction material processing system according to claim 1, characterized in that: The palladium-carbon preparation kettle (1) is provided with a vacuum delivery pipeline connected to the vacuum system of the hydrogenation reaction kettle (2).

4. A palladium-carbon catalytic hydrogenation reaction material processing system according to claim 1, characterized in that: The filter press cylinder (4) comprises a structure in which multiple layers of filter cloth and filter plates are alternately arranged.

5. A palladium-carbon catalytic hydrogenation reaction material processing system according to claim 1, characterized in that: The bottom of the hydrogenation reaction kettle (2) is provided with a conical flow guide structure, the cone angle is 60°, and the inner wall polishing roughness Ra≤0.4 μm.

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