Activity evaluation device and method for preparing aromatic thioamide catalyst using H2S

Abstract

The present invention relates to an activity evaluation device for preparing an aromatic thioamide catalyst using H2S, comprising a gas supply system, a conveying device, a reactor, a heating circulator, a product collector and a detection system; the gas supply system is connected to the gas inlet of the reactor, the heating circulator is connected to the insulation jacket of the reactor, the product collector is connected to the liquid outlet of the reactor, the detection system is connected to the end of the gas outlet pipeline of the reactor, and the conveying device is connected to the reaction material inlet of the reactor. The device overcomes the shortcomings of the reactor in the prior art that the reactor cannot be continuously produced, has high safety risks, is difficult to generate products and subsequently process the products, and the conventional catalysts are easily sulfated and deactivated due to salt accumulation on the surface.

Description

Technical Field

[0001] The invention relates to an activity evaluation device and method for preparing an aromatic thioamide catalyst by utilizing H2S, and belongs to the field of activity evaluation of sulfur high-value catalysts. Background Art

[0002] Hydrogen sulfide (H2S) is a highly toxic gas produced in the chemical production process using coal, oil and natural gas as raw materials. It not only corrodes pipelines and chemical production equipment, poisons and deactivates downstream catalysts, but also seriously pollutes the environment and harms human health. At present, the more mature technology for treating H2S is the Claus process. However, this process can only catalytically convert H2S into sulfur with low added value, while the H element contained is converted into H2O and discharged as wastewater, which not only pollutes the environment, but also loses a large amount of precious hydrogen resources. Therefore, it is urgent to develop a new technology that can efficiently treat H2S and realize the high-value utilization of H2S.

[0003] In fact, the molar content of hydrogen atoms in H2S is as high as ca. 66.7%. Compared with hydrogen, H2S is cheaper to use directly as a "hydrogen donor" and can also be used as a "sulfur donor" to achieve atomic economy and convert H and S elements in H2S into high value-added sulfur-containing chemicals. The key lies in building a feasible new chemical reaction system and designing new reaction equipment and catalysts.

[0004] Arylthioamides and their derivatives are an important class of organic compounds with broad application prospects in the fields of fine chemicals, biomedicine, polymer materials, etc. At present, the more commonly used method for synthesizing aromatic thioamides is to use aromatic nitriles or amides and sulfurizing agents such as carbon disulfide and hexamethyldisilathane to carry out the reaction of sulfur replacing oxygen. However, the atomic utilization rate of this technology is low, and it is easy to produce highly toxic waste gas, wastewater, and smelly sulfur byproducts during the reaction. Another method is to use H2S and aromatic nitriles to undergo nucleophilic addition reaction to synthesize thioamide compounds. This reaction can not only achieve the green conversion of H2S, but also simultaneously utilize the "hydrogen resources" in H2S, atomically economically utilize every atom in the H2S molecule, and achieve "near-zero waste emissions". However, the more difficult problem in the synthesis of thioamides in the existing technology is that the reaction device has the defects of poor production stability and low safety. The disadvantages of this technology are that the existing device is an intermittent reactor, which cannot be produced continuously, has high reaction pressure, poor corrosion resistance, high safety risks, and leads to product aggregation and increase of by-products as the reaction proceeds, which affects the formation of the product and the difficulty of subsequent product processing. Therefore, designing and developing a new device that can realize continuous synthesis of aromatic thioamide compounds is one of the important technical problems that need to be solved urgently.

[0005] At present, no relevant catalysts have been reported for the synthesis technology of thioamides by nucleophilic addition of H2S to aromatic nitrile. For this reaction, the intermediate reaction steps undergo the adsorption, activation, dissociation of H2S and aromatic nitrile compounds, and product desorption. From the perspective of these complex intermediate reaction processes, there are two main difficulties in the preparation of thioamides by nucleophilic addition of H2S to aromatic nitrile: (1) The sulfur atom in H2S can easily poison the metal active center, causing the desorption energy barrier of the sulfur intermediate at the active site to remain high, making it difficult to desorb and dissociate from the catalyst, resulting in low catalytic efficiency; (2) The strong oxidizing property of conventional metal oxide materials can easily cause the reaction system to form sulfate, resulting in salt deposition on the catalyst surface and deactivation. Therefore, another key is to design and prepare a new and efficient catalyst to promote this reaction.

[0006] Based on the above research, by designing a new device that can realize the continuous synthesis of aromatic thioamide compounds and designing a high-performance catalyst system, a new atom-economic reaction method for efficient catalytic conversion of H2S at the source is developed, providing a theoretical basis and technical source for the efficient removal and high-value utilization of H2S. Summary of the invention

[0007] In view of the deficiencies in the prior art, the technical problem to be solved by the present invention is to provide an activity evaluation device and method for preparing an aromatic thioamide catalyst using H2S.

[0008] In order to solve the above technical problems, the technical solution of the present invention is: an activity evaluation device for preparing aromatic thioamide catalyst using H2S, comprising a gas supply system, a conveying device, a reactor, a heating circulator, a product collector and a detection system; the gas supply system is connected to the gas inlet of the reactor, the heating circulator is connected to the insulation jacket of the reactor, the product collector is connected to the liquid outlet of the reactor, the detection system is connected to the end of the gas outlet pipeline of the reactor, and the conveying device is connected to the reaction material inlet of the reactor.

[0009] Preferably, the gas supply system includes a separate N2 gas source and a H2S / N2 balance gas source; the N2 concentration in the gas supply system is 95~100 wt%, and the H2S concentration is 0.05~5 wt%; the N2 in the gas supply system is used as the balance gas composition of H2S / N2 on the one hand, and a separate high-purity gas is used as the purge gas on the other hand.

[0010] Preferably, the delivery device includes a solvent delivery pump and a solute delivery pump; the solvent in the solvent delivery pump includes N,N-methylformamide, N,N-methylacetamide, ethylenediamine, and dimethyl sulfoxide, and the solute in the solute delivery pump includes p-toluenenitrile, p-nitrobenzonitrile, p-chlorobenzonitrile, p-bromobenzonitrile, p-iodobenzonitrile, p-nitrileacetophenone, and p-aminobenzonitrile.

[0011] Preferably, the upper kettle cover of the reactor is made of HC276 material, and the lower kettle body of the reactor is made of HC276 material and quartz material, and the whole is a cylindrical structure.

[0012] Preferably, the separate N2 gas source and H2S / N2 balancing gas source of the gas supply system are respectively connected to the three-way valve via pipelines, and are connected to the gas inlet of the reactor after being controlled by the three-way valve, wherein a pressure reducing valve and a filter are sequentially provided along the gas flow direction of the pipeline of the H2S / N2 balancing gas source, and a pressure reducing valve is provided on the pipeline of the N2 gas source.

[0013] Preferably, the heating circulator consists of internal and external circulations, and is provided with a liquid inlet and a liquid outlet. The external circulation pump of the heating circulator is connected to the external circulation, and the liquid outlet is connected to the inlet of the insulation jacket of the reactor with a high-temperature resistant hose, and the liquid inlet is connected to the outlet of the insulation jacket of the reactor.

[0014] Preferably, a ball valve is provided on the connecting pipeline between the conveying device and the reactor for adjusting the output flow rate of the pump; an agitator is provided in the reactor, and the stirring speed is 150~1000 r / min; a back pressure valve is provided on the gas outlet pipeline for adjusting the reaction pressure of the reactor, and a filter is provided for purifying the reaction gas; the gas after the reaction enters the detection system, and the type and concentration of the gas after the reaction can be detected; the solution after the reaction is transferred to the detection system, and the distribution and concentration of the reactants and products after the reaction can be detected; an exhaust gas treatment device is connected to the pipeline between the detection system and the corresponding filter.

[0015] An activity evaluation method for an activity evaluation device for preparing an aromatic thioamide catalyst using H2S comprises the following steps: 1) conveying a certain amount of solvent and aromatic nitrile compound into a reaction kettle, and purging with high-purity N2 to obtain pretreated solvent and reaction substrate, and preheating the purified solvent and reaction substrate; 2) contacting the purified aromatic nitrile compound with a catalyst to convert the aromatic nitrile compound into aromatic thioamide, and measuring the contents of the aromatic nitrile compound and aromatic thioamide after the reaction; 3) contacting the reacted H2S with a dehydrating agent to eliminate water and impurities in the reaction system, obtaining purified reaction gas, and measuring the H2S content in the purified reaction gas.

[0016] Preferably, in step 2), the catalyst after the reaction is separated from the reaction mixture, and sequentially subjected to N2 purging, distilled water washing, and drying regeneration processes to obtain a regenerated catalyst, and the catalytic performance of the regenerated catalyst for preparing aromatic thioamides is measured again.

[0017] Preferably, the application conditions for the nucleophilic addition of H2S to aromatic nitrile compounds to form thioamides are as follows: the feed gas flow rate is 10-50 mL / min, the purge gas nitrogen flow rate is 20-60 mL / min, the reaction temperature is 40-180 °C, the heating rate is 2-5 °C / min, the reaction solvent content is 80-95 wt.%, the reaction solute content is 5-20 wt.%, and the catalyst regeneration temperature is 180-220 °C.

[0018] Compared with the prior art, the present invention has the following beneficial effects:

[0019] 1. The present invention provides an activity evaluation device for continuously preparing aromatic thioamide catalysts using H2S in an atom-economic manner, comprising a gas supply system, a conveying device, a reactor, a heating circulator and a detection system. By connecting the gas supply system to the reactor, H2S can be introduced into the reactor to continuously react with aromatic nitrile compounds, so that aromatic thioamide can be continuously synthesized and continuously produced, and the generated products can be continuously separated from the reaction system, so that the raw materials can fully react and the generation of by-products can be suppressed, thereby achieving efficient preparation of aromatic thioamides with high product yield and good quality.

[0020] 2. The activity evaluation device for continuously preparing aromatic thioamide catalysts using H2S in an atom-economic manner provided by the present invention has advanced technology, low investment cost, high process safety, and can operate continuously and stably.

[0021] 3. The present invention provides an atomic-economical process for continuously preparing aromatic thioamides using H2S. It innovatively proposes to use H2S as a "hydrogen donor" and a "sulfur donor". It is a new atomic-economical process for the nucleophilic addition of H2S to aromatic nitrile compounds to prepare thioamides. It simultaneously achieves the source removal of H2S and the high-value utilization of H2S. In addition, the process does not produce wastewater such as H2O, and the process route is green and environmentally friendly.

[0022] The present invention is further described in detail below with reference to the accompanying drawings and specific embodiments. BRIEF DESCRIPTION OF THE DRAWINGS

[0023] Figure 1 Schematic diagram of the structure of an embodiment of the present invention.

[0024] In the figure: 1-gas supply system; 2-reactor; 3-heating circulator; 4-insulation jacket; 5-delivery pump; 6-agitator; 7-pressure gauge; 8-product collector; 9-three-way valve; 10-back pressure valve; 11-filter; 12-detection system; 13-six-way valve; 14-exhaust gas treatment device. DETAILED DESCRIPTION

[0025] The present invention will be further described below in conjunction with the accompanying drawings and embodiments.

[0026] It should be noted that the following detailed descriptions are exemplary and are intended to provide further explanation of the present application. Unless otherwise specified, all technical and scientific terms used herein have the same meanings as those commonly understood by those skilled in the art to which the present application belongs.

[0027] It should be noted that the terms used herein are only for describing specific embodiments and are not intended to limit the exemplary embodiments according to the present application. As used herein, unless the context clearly indicates otherwise, the singular form is also intended to include the plural form. In addition, it should be understood that when the terms "comprise" and / or "include" are used in this specification, it indicates the presence of features, steps, operations, devices, components and / or combinations thereof.

[0028] like Figure 1 As shown, this embodiment provides an activity evaluation device for preparing aromatic thioamide catalyst using H2S, including a gas supply system, a conveying device, a reactor, a heating circulator, a product collector and a detection system; the gas supply system is connected to the gas inlet of the reactor, the heating circulator is connected to the insulation jacket of the reactor, the product collector is connected to the liquid outlet of the reactor, the detection system is connected to the end of the gas outlet pipeline of the reactor, and the conveying device is connected to the reaction material inlet of the reactor. It overcomes the shortcomings of the reactor in the prior art that it cannot be continuously produced, has high safety risks, is difficult to generate products and subsequent product processing, and the existing conventional catalysts are easily sulfated and deactivated by surface salt accumulation.

[0029] In the embodiment of the present invention, the detection system includes gas detection units such as H2S, SO2, COS, CO2, and detection units for aromatic nitrile compounds, aromatic thioamide compounds and their derivatives, wherein the detection unit includes a six-way valve, an exhaust gas treatment device, a chromatographic analysis column, and the like.

[0030] In an embodiment of the present invention, the reactor is composed of an upper reactor cover, a lower reactor body, an agitator, a temperature measuring and controlling device, and a safety explosion device. The upper reactor cover is equipped with a liquid phase valve, a gas phase valve, a temperature measuring and controlling device, a safety explosion device, etc., and external valves, pressure gauges, etc. are directly connected through a ferrule; the valve is a ball valve or a needle valve; the agitator is a magnetic agitator, which is mainly made of stainless steel and NdFeB magnetic materials. Its specific working principle is that the external magnetic steel body is driven by a motor to rotate, and the external magnetic steel body drives the internal magnetic steel body, the stirring shaft and the stirring blades to rotate through the magnetic lines; the safety explosion device is a pressure relief safety device composed of a safety valve or a bursting disc holder. The gas phase valve is used for air intake, exhaust and vacuum, and the reactor also has a liquid phase valve for sampling and discharging; the product collector is a liquid collection tank for aromatic thioamide compounds and their derivatives, the inlet of which is connected to the discharge port (liquid outlet) of the liquid phase valve of the reactor, wherein the collection tank is also connected to the N2 gas valve of the gas supply system for purging the product of the collection tank. The aromatic thioamide compounds are p-tolylthioamide, p-nitrobenzylthioamide, p-chlorobenzylthioamide, p-bromobenzylthioamide, p-iodobenzylthioamide, p-ethylketonebenzylthioamide, p-aminobenzylthioamide, etc.

[0031] In an embodiment of the present invention, the heating circulator is equipped with a temperature control system, and the precise temperature correction function can reach 0.01 °C; when the working temperature of the heating circulator is 0-80 °C, the working medium is pure water; when the working temperature of the heating circulator is 80-100 °C, the working medium is an oil-water mixture; when the working temperature of the heating circulator is 100-180 °C, the working medium is oil.

[0032] In an embodiment of the present invention, the gas supply system includes a separate N2 gas source and a H2S / N2 balance gas source; the N2 concentration in the gas supply system is 95~100 wt%, and the H2S concentration is 0.05~5 wt%; in the gas supply system, N2 is used as the balance gas of H2S / N2 on the one hand, and a separate high-purity gas is used as the purge gas on the other hand.

[0033] In an embodiment of the present invention, the delivery device includes a solvent delivery pump and a solute delivery pump; the solvent in the solvent delivery pump includes N,N-methylformamide, N,N-methylacetamide, ethylenediamine, and dimethyl sulfoxide, and the solute in the solute delivery pump includes p-toluenenitrile, p-nitrobenzonitrile, p-chlorobenzonitrile, p-bromobenzonitrile, p-iodobenzonitrile, p-nitrileacetophenone, and p-aminobenzonitrile.

[0034] In the embodiment of the present invention, the upper kettle cover of the reactor is made of HC276 material, and the lower kettle body of the reactor is made of HC276 material and quartz material, and the whole is a cylindrical structure.

[0035] In an embodiment of the present invention, the separate N2 gas source and H2S / N2 balancing gas source of the gas supply system are respectively connected to the three-way valve via pipelines, and are connected to the gas inlet of the reactor after being controlled by the three-way valve, wherein a pressure reducing valve, a pressure gauge, and a filter are sequentially provided along the gas flow direction of the pipeline of the H2S / N2 balancing gas source for gas purification, and a pressure reducing valve and a pressure gauge are provided on the pipeline of the N2 gas source.

[0036] In an embodiment of the present invention, the heating circulator is composed of internal and external circulations, and is provided with a liquid inlet and a liquid outlet. The external circulation pump of the heating circulator is connected to the external circulation, and the liquid outlet is connected to the inlet of the insulation jacket of the reactor with a high-temperature resistant hose, and the liquid inlet is connected to the outlet of the insulation jacket of the reactor.

[0037] In an embodiment of the present invention, the inlet of the conveying device is connected to the reaction material pipeline, and the outlet of the conveying device is connected to the reaction material inlet of the reactor. The volume of the reactor is 100 mL, and the height-to-diameter ratio of the reactor is 3:1. A ball valve is provided on the connecting pipeline between the conveying device and the reactor to adjust the output flow of the pump; an agitator is provided in the reactor, and the stirring speed is 150~1000 r / min; a back pressure valve is provided on the gas outlet pipeline to adjust the reaction pressure of the reactor, and a filter is provided for purifying the reaction gas; the gas after the reaction enters the detection system, and the type and concentration of the gas after the reaction can be detected. The solution after the reaction is transferred to the detection system, and the distribution and concentration of the reactants and products after the reaction can be detected; the pipeline between the detection system and the corresponding filter is connected to an exhaust gas treatment device.

[0038] In the embodiment of the present invention, the reaction temperature of the reactor is 25-180 ° C, and the reaction pressure is 0-2 Mpa;

[0039] An activity evaluation method for an activity evaluation device for preparing an aromatic thioamide catalyst using H2S comprises the following steps: 1) conveying a certain amount of solvent and aromatic nitrile compound into a reaction kettle, and purging with high-purity N2 to obtain pretreated solvent and reaction substrate, and preheating the purified solvent and reaction substrate; 2) contacting the purified aromatic nitrile compound with a catalyst to convert the aromatic nitrile compound into aromatic thioamide, and measuring the contents of the aromatic nitrile compound and aromatic thioamide after the reaction; 3) contacting the reacted H2S with a dehydrating agent to eliminate water and impurities in the reaction system, obtaining purified reaction gas, and measuring the H2S content in the purified reaction gas.

[0040] In the embodiment of the present invention, in step 2), the catalyst after the reaction is separated from the reaction mixture, and sequentially subjected to N2 purging, distilled water washing, and drying regeneration processes to obtain a regenerated catalyst, and the catalytic performance of the regenerated catalyst for preparing aromatic thioamides is measured again.

[0041] In an embodiment of the present invention, the application conditions for the nucleophilic addition of H2S to an aromatic nitrile compound to form a thioamide reaction are as follows: a raw gas flow rate of 10-50 mL / min, a purge gas nitrogen flow rate of 20-60 mL / min, a reaction temperature of 40-180 °C, a heating rate of 2-5 °C / min, a reaction solvent content of 80-95 wt.%, a reaction solute content of 5-20 wt.%, and a catalyst regeneration temperature of 180-220 °C.

[0042] Specific implementation process:

[0043] Example 1

[0044] This embodiment provides an activity evaluation method for continuously preparing an aromatic thioamide catalyst using H2S by atom economy, comprising the following steps:

[0045] First, fill the reactor with a catalyst (the powder particle size of the catalyst is 250-300 mesh, and the catalyst can be but not limited to metal Fe, Co, Cu, Ni, Mo, Ru, etc., loaded on MgAl2O4, Al2O3, Fe2O3, CeO2, MgO2, MoS2, V2O5, g-C3N4, and various nitrogen-doped carbon carriers). Catalytic materials), then under the protection of a nitrogen atmosphere, the solvent N,N-methylformamide is delivered to the reactor by a solvent delivery pump and the solute benzonitrile is delivered to the reactor by a solute delivery pump at a molar ratio of 10:1 through a material pipeline. Start the agitator and set the speed to 300-1000 r / min, start the heating circulator and adjust the temperature to 60-120 ° C. After the stirring speed and temperature are stable, the reaction gas is introduced into the reaction device through the H2S / N2 inlet pipeline, and the pressure is set to 0.5-1.8 Mpa through the back pressure valve. After the reaction is stable, observe the changes in the material in the reactor, use the chromatogram to observe the composition and concentration of the gas online, and the detected gas can be subjected to tail gas absorption treatment by the tail gas treatment device, and emptied after the tail gas absorption treatment. After the reaction is completely completed, the H2S / N2 gas circuit is switched to a high-purity N2 pipeline to purge the reactor and the pipeline, and the reaction product is collected by a product collector, and the collected product is centrifuged and statically layered to obtain an aromatic thioamide compound, and its content is analyzed by chromatography. After testing, the activity evaluation test of the H2S nucleophilic addition aromatic nitrile group thioamide catalyst is completed by the method in this embodiment, that is, the device can achieve the purpose of quickly and stably screening different types of sulfur high-value catalysts.

[0046] Example 2

[0047] This embodiment provides an activity evaluation method for continuously preparing an aromatic thioamide catalyst using H2S by atom economy, comprising the following steps:

[0048] First, fill the reactor with a catalyst (the powder particle size of the catalyst is 250-300 meshes, and the catalyst can be, but is not limited to, metal Fe, Co, Cu, Ni, Mo, Ru, etc., loaded on MgAl2O4, Al2O3, Fe2O3, CeO2, MgO2, MoS2, V2O5, g-C3N4, and various nitrogen-doped carbon carriers. Catalytic materials), then under the protection of a nitrogen atmosphere, the solvent N, N-methylacetamide is delivered to the reactor by a solvent delivery pump and the solute p-chlorobenzonitrile is delivered to the reactor by a material pipeline at a molar ratio of 10:1 by a solute delivery pump. Start the agitator and set the speed to 300-1000 r / min, start the heating circulator and adjust the temperature to 60-120 ° C. After the stirring speed and temperature are stable, the reaction gas is introduced into the reaction device through the H2S / N2 inlet pipeline, and the pressure is set to 0.5-1.8 Mpa through the back pressure valve. After the reaction is stable, observe the changes in the material in the reactor, use the chromatogram to observe the composition and concentration of the gas online, and the detected gas can be subjected to tail gas absorption treatment by the tail gas treatment device, and emptied after the tail gas absorption treatment. After the reaction is completely completed, the H2S / N2 gas circuit is switched to a high-purity N2 pipeline to purge the reactor and the pipeline, and the reaction product is collected by a product collector, and the collected product is centrifuged and statically layered to obtain an aromatic thioamide compound, and its content is analyzed by chromatography. After testing, the activity evaluation test of the H2S nucleophilic addition aromatic nitrile group thioamide catalyst is completed by the method in this embodiment, that is, the device can achieve the purpose of quickly and stably screening different types of sulfur high-value catalysts.

[0049] Example 3

[0050] This embodiment provides an activity evaluation method for continuously preparing an aromatic thioamide catalyst using H2S by atom economy, comprising the following steps:

[0051] First, fill the reactor with a catalyst (the powder particle size of the catalyst is 250-300 mesh, and the catalyst can be but not limited to metal Fe, Co, Cu, Ni, Mo, Ru, etc., loaded on MgAl2O4, Al2O3, Fe2O3, CeO2, MgO2, MoS2, V2O5, g-C3N4, and various nitrogen-doped carbon carriers). Catalytic materials), then under the protection of a nitrogen atmosphere, the solvent dimethyl sulfoxide is delivered to the reactor by a solvent delivery pump and the solute p-aminobenzonitrile is delivered to the reactor by a solute delivery pump at a molar ratio of 10:1 through a material pipeline. Start the agitator and set the speed to 300-1000 r / min, start the heating circulator and adjust the temperature to 60-120 °C. After the stirring speed and temperature are stable, the reaction gas is introduced into the reaction device through the H2S / N2 inlet pipeline, and the pressure is set to 0.5-1.8 Mpa through the back pressure valve. After the reaction is stable, the changes in the materials in the reactor are observed, and the composition and concentration of the gas are detected online by gas chromatography. The gas after detection can be subjected to tail gas absorption treatment by the tail gas treatment device, and the tail gas absorption treatment is emptied. After the reaction is completely completed, the H2S / N2 gas circuit is switched to a high-purity N2 pipeline to purge the reactor and the pipeline, and the reaction product is collected by a product collector, and the collected product is centrifuged and statically layered to obtain an aromatic thioamide compound, and its content is analyzed by chromatography. After testing, the activity evaluation test of the catalyst for preparing thioamide by the nucleophilic addition of aromatic nitrile groups of H2S is completed by the method in the present embodiment, that is, the device can achieve the purpose of quickly and stably screening different types of sulfur high-value catalysts.

[0052] The above is only a preferred embodiment of the present invention, and does not limit the present invention in other forms. Any technician familiar with the profession may use the above disclosed technical content to change or modify it into an equivalent embodiment with equivalent changes. However, any simple modification, equivalent change and modification made to the above embodiment according to the technical essence of the present invention without departing from the technical solution of the present invention still belongs to the protection scope of the technical solution of the present invention.

Claims

1. An activity evaluation method for an activity evaluation device for preparing an aromatic thioamide catalyst using H2S, characterized in that: The device comprises a gas supply system, a conveying device, a reactor, a heating circulator, a product collector and a detection system; the gas supply system is connected to the gas inlet of the reactor, the heating circulator is connected to the insulation jacket of the reactor, the product collector is connected to the liquid outlet of the reactor, the detection system is connected to the end of the gas outlet pipeline of the reactor, and the conveying device is connected to the reaction material inlet of the reactor; the gas supply system comprises a separate N2 gas source and a balanced H2S / N2 gas source; the N2 concentration in the gas supply system is 95-100 wt%, and the H2S concentration is 0.05-5 wt%; in the gas supply system, N2 is used as the balance gas of H2S / N2 on the one hand, and a separate high-purity gas is used as the purge gas on the other hand; the delivery device includes a solvent delivery pump and a solute delivery pump; the solvent in the solvent delivery pump includes N,N-methylformamide, N,N-methylacetamide, ethylenediamine, and dimethyl sulfoxide, and the solute in the solute delivery pump includes p-toluene nitrile, p-nitrobenzonitrile, p-chlorobenzonitrile, p-bromobenzonitrile, p-iodobenzonitrile, p-nitrile acetophenone, and p-aminobenzonitrile; the method includes the following steps: 1) adding a certain The invention relates to the following steps: 1) conveying a large amount of solvent and aromatic nitrile compound to a reactor, and purging with high-purity N2 to obtain pretreated solvent and reaction substrate, and preheating the purified solvent and reaction substrate; 2) contacting the purified aromatic nitrile compound with a catalyst to convert the aromatic nitrile compound into aromatic thioamide, and determining the contents of the aromatic nitrile compound and aromatic thioamide after the reaction; 3) contacting the reacted H2S with a dehydrating agent to eliminate water and impurities in the reaction system to obtain purified reaction gas, and determining the content of H2S in the purified reaction gas.

2. The activity evaluation method of the activity evaluation device for preparing an aromatic thioamide catalyst using H2S according to claim 1, characterized in that: The upper kettle cover of the reactor is made of HC276 material, and the lower kettle body of the reactor is made of HC276 material and quartz material, and the whole is a cylindrical structure.

3. The activity evaluation method of the activity evaluation device for preparing an aromatic thioamide catalyst using H2S according to claim 1, characterized in that: The separate N2 gas source and H2S / N2 balancing gas source of the gas supply system are respectively connected to the three-way valve via pipelines, and are connected to the gas inlet of the reactor after being controlled by the three-way valve, wherein a pressure reducing valve and a filter are sequentially arranged along the gas flow direction of the pipeline of the H2S / N2 balancing gas source, and a pressure reducing valve is arranged on the pipeline of the N2 gas source.

4. The activity evaluation method of the activity evaluation device for preparing an aromatic thioamide catalyst using H2S according to claim 1, characterized in that: The heating circulator consists of internal and external circulations, and is provided with a liquid inlet and a liquid outlet. The external circulation pump of the heating circulator is connected to the external circulation, and the liquid outlet is connected to the insulation jacket inlet of the reactor with a high-temperature resistant hose, and the liquid inlet is connected to the insulation jacket outlet of the reactor.

5. The activity evaluation method of the activity evaluation device for preparing aromatic thioamide catalyst using H2S according to claim 1, characterized in that: A ball valve is provided on the connecting pipeline between the conveying device and the reactor for adjusting the output flow of the pump; an agitator is provided in the reactor, and the stirring speed is 150~1000 r / min; a back pressure valve is provided on the gas outlet pipeline for adjusting the reaction pressure of the reactor, and a filter is provided for purifying the reaction gas; the gas after the reaction enters the detection system, and the type and concentration of the gas after the reaction can be detected; the solution after the reaction is transferred to the detection system, and the distribution and concentration of the reactants and products after the reaction can be detected; an exhaust gas treatment device is connected to the pipeline between the detection system and the corresponding filter.

6. The activity evaluation method of the activity evaluation device for preparing aromatic thioamide catalyst using H2S according to claim 1, characterized in that: In step 2), the catalyst after the reaction is separated from the reaction mixture, and is successively subjected to N2 purging, distilled water washing, and drying regeneration processes to obtain a regenerated catalyst, and the catalytic performance of the regenerated catalyst for preparing aromatic thioamides is measured again.

7. The activity evaluation method of the activity evaluation device for preparing aromatic thioamide catalyst using H2S according to claim 1, characterized in that: The application conditions for the nucleophilic addition of H2S to aromatic nitrile compounds to form thioamide reaction are as follows: the feed gas flow rate is 10-50 mL / min, the purge gas nitrogen flow rate is 20-60 mL / min, the reaction temperature is 40-180 °C, the heating rate is 2-5 °C / min, the reaction solvent content is 80-95 wt.%, the reaction solute content is 5-20 wt.%, and the catalyst regeneration temperature is 180-220 °C.

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