Reaction-extraction experimental device

Abstract

The utility model discloses a reaction-extraction experimental device which comprises a formylation reaction kettle, an extraction container and a hydrogenation reaction kettle, wherein a discharge valve at the bottom of the formylation reaction kettle is connected to a feed port at the top of the extraction container; a discharge valve at the bottom of the extraction container is respectively connected to a feed port at the top of the formylation reaction kettle, a feed port at the top of the hydrogenation reaction kettle and a first waste liquid collecting barrel, and a discharge valve at the bottom of the hydrogenation reaction kettle is connected to a second waste liquid collecting barrel; gas source pipelines and emptying pipelines are arranged at the tops of the formylation reaction kettle, the extraction container and the hydrogenation reaction kettle, pinhole valves are arranged on the gas source pipelines of the formylation reaction kettle, the extraction container and the hydrogenation reaction kettle, and pinhole valves are arranged on the emptying pipelines of the formylation reaction kettle, the extraction container and the hydrogenation reaction kettle; balances are arranged at the bottoms of the formylation reaction kettle and the hydrogenation reaction kettle. The device is used for formylation reaction in a laboratory and can be applied to other reaction-extraction processes at the same time.

Description

Technical Field

[0001] The utility model relates to an experimental device, more specifically, to a reaction-extraction experimental device. Background Art

[0002] Carbonylation reaction is a type of reaction that introduces CO and other groups into organic compound molecules to synthesize target products. It mainly includes hydroformylation, hydrocarboxylation and hydroesterification.

[0003] The hydroformylation reaction of olefins is a reaction in which olefins react with synthesis gas under the action of a catalyst to produce aldehydes with one carbon atom higher than the raw olefins. Since the discovery of the hydroformylation reaction, it has become an important organic chemical process in petrochemical production. The annual production of aldehydes and alcohols is nearly 10mt and is widely used in fine chemical fields such as plasticizers, surfactants, pharmaceutical intermediates, solvents and fragrances.

[0004] The process of hydroesterification reaction mainly includes the hydroesterification reaction of styrene and the hydroesterification reaction used in the preparation of 3-hydroxycarboxylic acid esters. The preparation of carboxylic acid esters by hydroesterification of ethylene is a chemical reaction with broad application prospects. The ester compounds produced are widely used in the wine, food, cosmetics and other industries. 3-Hydroxycarboxylic acid esters are important organic synthesis intermediates generated by carbonylation reaction of ethylene oxide (EO) as raw material with methanol and carbon monoxide. They are widely used in the synthesis of organic fine chemicals, medicines, pesticide intermediates, etc.

[0005] Hydrocarboxylation reaction mainly includes the synthesis of acetic acid, phenylacetic acid and naphthylacetic acid from methanol carbonylation. As an important basic organic chemical raw material, acetic acid and acetic anhydride, phenylacetic acid, naphthylacetic acid and their downstream derivatives are widely used in the synthesis of medicine, synthetic fiber, textile, leather, pesticide, rubber and metal processing, food and fine chemicals.

[0006] Our company uses rhodium ion solution as a catalyst and phosphorus compounds as ligands, and has various applications in the formylation process through different catalyst systems. For example, the butyl octanol workshop uses propylene as a raw material to react with synthesis gas, and then uses a heat exchanger and a tower to separate the product. There is also an acetic acid workshop that uses methanol as a raw material and uses rhodium catalysts and carbon monoxide to synthesize acetic acid. Based on our company's various applications of formylation reactions, and in order to improve the process and explore new production methods, there is a certain demand for conducting small-scale experimental reactions to generate products and analyze their product content. While collecting data, we also summarize and verify the laws and characteristics of different formylation reactions, and demonstrate the feasibility of improvements.

[0007] However, during the experiment, there are several problems:

[0008] (1) The mass changes of synthesis gas and hydrogen consumption cannot be accurately measured due to factors such as solution adhesion to the wall;

[0009] (2) The reaction starts with formylation and ends with hydrogenation of organic aqueous solution, which is a complicated operation;

[0010] (3) The entire process contains toxic substances and may even involve contact with highly toxic substances, posing a risk of poisoning. Utility Model Content

[0011] The purpose of the utility model is to overcome the deficiencies in the prior art and propose a reaction-extraction experimental device. The utility model reduces the risk of poisoning caused by leakage of toxic substances by connecting the pipelines of the reaction container in a sealed manner, and installs a balance to monitor the change of reaction quality in real time, so that the experimental results are more accurate and more meaningful for reference. The purpose of the utility model is achieved through the following technical solutions.

[0012] The purpose of the utility model is achieved through the following technical solutions.

[0013] The utility model reaction-extraction experimental device comprises a formylation reactor, an extraction container and a hydrogenation reactor. The discharge valve at the bottom of the formylation reactor is connected to the feed port at the top of the extraction container through a pipeline. The discharge valve at the bottom of the extraction container is respectively connected to the feed port at the top of the formylation reactor, the feed port at the top of the hydrogenation reactor and a first waste liquid collection bucket through pipelines. The discharge valve at the bottom of the hydrogenation reactor is connected to the second waste liquid collection bucket through a pipeline. The formylation reactor, the extraction container and the hydrogenation reactor are all provided with a gas source pipeline and a venting pipeline at the top. The gas source pipelines at the tops of the formylation reactor, the extraction container and the hydrogenation reactor are respectively provided with an eleventh pinhole valve, a twelfth pinhole valve and a thirteenth pinhole valve. The venting pipelines at the tops of the formylation reactor, the extraction container and the hydrogenation reactor are respectively provided with a first pinhole valve, a second pinhole valve and a third pinhole valve. The formylation reactor and the hydrogenation reactor are respectively provided with a first balance and a second balance at the bottom.

[0014] In the above device, the formylation reactor, extraction container and hydrogenation reactor are respectively provided with a detachable first reactor jacket, a second reactor jacket and a third reactor jacket integrated with stirring and heating on the outside, and are respectively provided with a first rotor, a second rotor and a third rotor for stirring on the inside; the outer sides of the formylation reactor and the hydrogenation reactor are provided with brackets, which are respectively fixed to the first level and the second level through the brackets.

[0015] In the above device, the formylation reactor is composed of a stainless steel cylindrical body and a stainless steel cover. The bottom of the stainless steel cylindrical body is an arc bottom and is equipped with a discharge valve. A first PTFE gasket is arranged between the top of the stainless steel cylindrical body and the stainless steel cover and is fastened by bolts.

[0016] In the above device, the extraction container is composed of a transparent glass cylindrical body and a glass cover. The bottom of the glass cylindrical body is an arc bottom and is equipped with a discharge valve. A third tetrafluoro gasket is arranged between the top of the glass cylindrical body and the glass cover and is fastened by bolts.

[0017] In the above device, the hydrogenation reactor is composed of a stainless steel cylindrical body and a stainless steel cover. The bottom of the stainless steel cylindrical body is an arc bottom and is equipped with a discharge valve. A second PTFE gasket is arranged between the top of the stainless steel cylindrical body and the stainless steel cover and is fastened by bolts.

[0018] In the above device, a fourth needle hole valve and a first clamping type vacuum quick release flange are arranged on the pipeline connecting the discharge valve at the bottom of the formylation reactor and the feed port at the top of the extraction container. The fourth needle hole valve is located at one end of the extraction container, and the first clamping type vacuum quick release flange is located at one end of the formylation reactor.

[0019] In the above device, a fifth needle hole valve and a second clamping type vacuum quick release flange are arranged on the pipeline connecting the discharge valve at the bottom of the extraction container and the feed port at the top of the formylation reactor, a sixth needle hole valve and a third clamping type vacuum quick release flange are arranged on the pipeline connecting the discharge valve at the bottom of the extraction container and the first waste liquid collection bucket, and a seventh needle hole valve and a fourth clamping type vacuum quick release flange are arranged on the pipeline connecting the discharge valve at the bottom of the extraction container and the feed port at the top of the hydrogenation reactor.

[0020] In the above-mentioned device, both the first waste liquid collection barrel and the second waste liquid collection barrel are provided with drain pipes, the drain pipe of the first waste liquid collection barrel is provided with a ninth needle hole valve and a sixth clamping type vacuum quick release flange, and the drain pipe of the second waste liquid collection barrel is provided with a tenth needle hole valve and a seventh clamping type vacuum quick release flange.

[0021] In the above device, a fifth clamping type vacuum quick release flange and an eighth needle hole valve are arranged on the pipeline connecting the bottom discharge valve of the hydrogenation reactor and the second waste liquid collection barrel. The fifth clamping type vacuum quick release flange is located at one end of the hydrogenation reactor, and the eighth needle hole valve is located at one end of the second waste liquid collection barrel.

[0022] Compared with the prior art, the beneficial effects brought about by the technical solution of the utility model are:

[0023] (1) The utility model connects three reactions into a set of devices and adopts a closed process, which reduces the risk of leakage and poisoning and improves safety.

[0024] (2) After the catalyst, solution, etc. are added, the utility model can realize the whole process operation only by opening and closing the valve, thus simplifying the operation steps.

[0025] (3) The utility model solves the problem that the mass change of synthesis gas and hydrogen consumption cannot be accurately measured due to factors such as solution wall adhesion, and the experimental results are more accurate.

[0026] (4) The utility model adopts a clamping type vacuum quick-release flange, which is convenient for disassembly and helps to adjust the direction of materials. On the other hand, in order to observe the quality changes of the kettle container, if it is necessary to eliminate the influence of metal pipeline stress, the flange can be disassembled to eliminate it. BRIEF DESCRIPTION OF THE DRAWINGS

[0027] Figure 1 It is a schematic diagram of the reaction-extraction experimental device of the utility model.

[0028] Figure numerals: 1-formylation reactor, 2-extraction container, 3-hydrogenation reactor, 4-first waste liquid collection barrel, 5-second waste liquid collection barrel, 6-first reactor jacket, 7-second reactor jacket, 8-third reactor jacket, 9-first rotor, 10-second rotor, 11-third rotor, 12-first balance, 13-second balance, 14-first gasket, 15-second gasket, 16-third gasket, 17-first needle hole valve, 18-second needle hole valve, 19-third needle hole valve, 20-fourth needle hole valve, 21-first clamping type vacuum Quick release flange, 22-fifth needle hole valve, 23-sixth needle hole valve, 24-seventh needle hole valve, 25-second clamping type vacuum quick release flange, 26-third clamping type vacuum quick release flange, 27-fourth clamping type vacuum quick release flange, 28-fifth clamping type vacuum quick release flange, 29-eighth needle hole valve, 30-sixth clamping type vacuum quick release flange, 31-seventh clamping type vacuum quick release flange, 32-ninth needle hole valve, 33-tenth needle hole valve, 34-eleventh needle hole valve, 35-twelfth needle hole valve, 36-thirteenth needle hole valve. DETAILED DESCRIPTION

[0029] The utility model is further described below in conjunction with the accompanying drawings.

[0030] like Figure 1As shown, the reaction-extraction experimental device of the utility model mainly includes a formylation reactor 1, an extraction container 2, a hydrogenation reactor 3, a first waste liquid collection barrel 4, a second waste liquid collection barrel 5, a first reactor jacket 6, a second reactor jacket 7, a third reactor jacket 8, a first rotor 9, a second rotor 10, a third rotor 11, a first balance 12, a second balance 13, a first gasket 14, a second gasket 15, a third gasket 16, a first needle hole valve 17, a second needle hole valve 18, a third needle hole valve 19, a fourth needle hole valve 20, a first clamping type vacuum The quick-release flange 21, the fifth needle hole valve 22, the sixth needle hole valve 23, the seventh needle hole valve 24, the second clamping type vacuum quick-release flange 25, the third clamping type vacuum quick-release flange 26, the fourth clamping type vacuum quick-release flange 27, the fifth clamping type vacuum quick-release flange 28, the eighth needle hole valve 29, the sixth clamping type vacuum quick-release flange 30, the seventh clamping type vacuum quick-release flange 31, the ninth needle hole valve 32, the tenth needle hole valve 33, the eleventh needle hole valve 34, the twelfth needle hole valve 35, the thirteenth needle hole valve 36 and related connecting pipelines.

[0031] The bottom discharge valve of the formylation reactor 1 is connected to the top feed port of the extraction container 2 through a pipeline, and the bottom discharge valve of the extraction container 2 is respectively connected to the top feed port of the formylation reactor 1, the top feed port of the hydrogenation reactor 3, and the first waste liquid collection bucket 4 through pipelines. Specifically, the pipeline of the bottom discharge valve of the extraction container 2 extends out to connect to the four-way, and the remaining three ports of the four-way are respectively connected to the top feed port of the formylation reactor 1, the top feed port of the hydrogenation reactor 3, and the first waste liquid collection bucket 4 through pipelines. The bottom discharge valve of the hydrogenation reactor 3 is connected to the second waste liquid collection bucket 5 through a pipeline.

[0032] The formylation reactor 1, extraction container 2, and hydrogenation reactor 3 are provided with a detachable first reactor jacket 6, a second reactor jacket 7, and a third reactor jacket 8 for stirring and heating, respectively, and the formylation reactor 1, extraction container 2, and hydrogenation reactor 3 are provided with a first rotor 9, a second rotor 10, and a third rotor 11 for stirring, respectively. The second reactor jacket 6 and the second rotor 9 constitute the heating and stirring device of the formylation reactor 1, the first reactor jacket 7 and the first rotor 10 constitute the heating and stirring device of the extraction container 2, and the third reactor jacket 8 and the third rotor 11 constitute the heating and stirring device of the hydrogenation reactor 3. The formylation reactor 1, extraction container 2, and hydrogenation reactor 3 are all provided with a gas source pipeline and a venting pipeline at the top, and the gas source pipelines at the top of the formylation reactor 1, extraction container 2, and hydrogenation reactor 3 convey different types of gases, and the first waste liquid collection barrel 4 and the second waste liquid collection barrel 5 are both provided with a venting pipeline. The gas sources of the formylation reactor 1 are nitrogen and synthesis gas, the gas source of the extraction container 2 is only nitrogen, and the gas sources of the hydrogenation reactor 3 are nitrogen and hydrogen. The gas source pipelines at the top of the formylation reactor 1, the extraction container 2, and the hydrogenation reactor 3 are respectively provided with an eleventh needle hole valve 34, a twelfth needle hole valve 35, and a thirteenth needle hole valve 36. The venting pipelines at the top of the formylation reactor 1, the extraction container 2, and the hydrogenation reactor 3 are respectively provided with a first needle hole valve 17, a second needle hole valve 18, and a third needle hole valve 19. The venting pipeline of the first waste liquid collection barrel 4 is provided with a ninth needle hole valve 32 and a sixth clamping type vacuum quick release flange 30, and the venting pipeline of the second waste liquid collection barrel 5 is provided with a tenth needle hole valve 33 and a seventh clamping type vacuum quick release flange 31.

[0033] In the above device, the outer sides of the formylation reactor 1 and the hydrogenation reactor 3 are provided with brackets (without affecting the reactor jacket and pipelines), which are respectively fixed to the first balance 12 and the second balance 13 through the brackets. The accuracy of the first balance 12 and the second balance 13 is required to be two decimal places or more.

[0034] In the above device, the formylation reactor 1 is composed of a stainless steel cylindrical body and a stainless steel cover. The bottom of the stainless steel cylindrical body is an arc bottom to prevent affecting the rotation of the rotor. A discharge valve (which does not affect the rotation of the rotor) is installed. A first polytetrafluoroethylene gasket 14 is arranged between the top of the stainless steel cylindrical body and the stainless steel cover and is fastened by bolts.

[0035] In the above device, the extraction container 2 is composed of a high-strength transparent glass cylindrical body and a glass cylinder cover. The bottom of the glass cylindrical body is an arc bottom to prevent affecting the rotation of the rotor. A discharge valve is installed (which does not affect the rotation of the rotor). A third tetrafluoro gasket 16 is arranged between the top of the glass cylindrical body and the glass cylinder cover and is fastened by bolts.

[0036] In the above device, the hydrogenation reactor 3 is composed of a stainless steel cylindrical body and a stainless steel cover. The bottom of the stainless steel cylindrical body is an arc bottom and is equipped with a discharge valve (which does not affect the rotation of the rotor). A second PTFE gasket 15 is arranged between the top of the stainless steel cylindrical body and the stainless steel cover and is fastened by bolts.

[0037] In the above device, a fourth needle hole valve 20 and a first clamping type vacuum quick release flange 21 are arranged on the pipeline connecting the bottom discharge valve of the formylation reactor 1 and the top feed port of the extraction container 2. The fourth needle hole valve 20 is as close to one end of the extraction container 2 as possible, and the first clamping type vacuum quick release flange 21 is as close to one end of the formylation reactor 1 as possible.

[0038] In the above device, the pipeline connecting the bottom discharge valve of the extraction container 2 and the top feed port of the formylation reactor 1 is provided with a fifth needle hole valve 22 and a second clamping type vacuum quick release flange 25, the pipeline connecting the bottom discharge valve of the extraction container 2 and the first waste liquid collection bucket 4 is provided with a sixth needle hole valve 23 and a third clamping type vacuum quick release flange 26, and the pipeline connecting the bottom discharge valve of the extraction container 2 and the top feed port of the hydrogenation reactor 3 is provided with a seventh needle hole valve 24 and a fourth clamping type vacuum quick release flange 27. The fifth needle hole valve 22, the sixth needle hole valve 23, the seventh needle hole valve 24, the second clamping type vacuum quick release flange 25, the third clamping type vacuum quick release flange 26, and the fourth clamping type vacuum quick release flange 27 are all as far away from one end of the extraction container 2 as possible.

[0039] In the above device, a fifth clamping type vacuum quick release flange 28 and an eighth needle hole valve 29 are provided on the pipeline connecting the bottom discharge valve of the hydrogenation reactor 3 and the second waste liquid collection barrel 5. The fifth clamping type vacuum quick release flange 28 is as close to one end of the hydrogenation reactor 3 as possible, and the eighth needle hole valve 29 is as close to one end of the second waste liquid collection barrel 5 as possible.

[0040] Before introducing the solution of the formylation reaction kettle 1 that has completed the formylation reaction into the extraction container 2, it should be ensured that all pipelines are closed except for the pipeline connecting the discharge valve at the bottom of the formylation reaction kettle 1 and the feed port at the top of the extraction container 2 and the venting pipeline of the extraction container 2. Specifically, the valves on the gas source pipelines of the formylation reaction kettle 1 and the extraction container 2 are all closed (i.e., the eleventh needle hole valve 34 and the twelfth needle hole valve 35 are closed), and the valve status is checked, wherein the first needle hole valve 17 and the fifth needle hole valve 22 are closed, the second needle hole valve 18 and the fourth needle hole valve 20 are opened, and the discharge valves of the formylation reaction kettle 1 and the extraction container 2 are closed. Open the discharge valve at the bottom of the formylation reaction kettle 1, slowly open the gas source of the formylation reaction kettle 1 (i.e., slowly open the eleventh needle hole valve 34), and start the introduction. Observe the liquid level of the extraction container 2. When the liquid level stops rising, close the gas source of the formylation reactor 1 (i.e., close the eleventh needle hole valve 34), close the bottom discharge valve of the formylation reactor 1, and close the second needle hole valve 18 and the fourth needle hole valve 20. At this time, the solution is introduced into the extraction container 2, and the valves on all pipelines of the two containers are closed.

[0041] Before introducing the aqueous solution in the extraction container 2 into the hydrogenation reactor 3, it should be ensured that all pipelines are closed except for the pipeline connecting the bottom discharge valve of the extraction container 2 and the top feed port of the hydrogenation reactor 3 and the venting pipeline of the hydrogenation reactor 3. Specifically, the valves on the gas source pipelines of the extraction container 2 and the hydrogenation reactor 3 are all closed (i.e., the twelfth needle hole valve 35 and the thirteenth needle hole valve 36 are closed), and the valve status is checked, wherein the second needle hole valve 18, the fourth needle hole valve 20, the fifth needle hole valve 22, and the sixth needle hole valve 23 are closed, the third needle hole valve 19 and the seventh needle hole valve 24 are opened, and the bottom discharge valves of the extraction container 2 and the hydrogenation reactor 3 are closed. Open the bottom discharge valve of the extraction container 2, slowly open the gas source of the extraction container 2 (i.e., slowly open the twelfth needle hole valve 35), and observe the liquid level of the extraction container 2. When the liquid level approaches the oil-water boundary, close the discharge valve at the bottom of the extraction container 2, close the seventh needle hole valve 24, and close the nitrogen gas source of the extraction container 2 (i.e., close the twelfth needle hole valve 35). Open the ninth needle hole valve 32, the sixth needle hole valve 23, open the discharge valve at the bottom of the extraction container 2, slowly open the gas source (i.e., slowly open the twelfth needle hole valve 35), and observe the liquid level of the extraction container 2 until the oil-water interface disappears. Close the gas source (i.e., close the twelfth needle hole valve 35), the discharge valve at the bottom of the extraction container 2, the ninth needle hole valve 32, and the sixth needle hole valve 23, and the remaining toluene solution is reused or discharged as needed.

[0042] The experimental processing process based on the above reaction-extraction experimental device is as follows:

[0043] (1) Use a pipette, an electronic balance, and a volumetric flask to prepare a solution with propylene alcohol as the solute and toluene as the solvent. Weigh the rhodium catalyst, triphenylphosphine ligand, deionized water, and an appropriate amount of Raney nickel catalyst. Confirm that all valves are closed, all containers are sealed, and the heating kettle jackets (i.e., the first kettle jacket 6 and the second kettle jacket 7) are in a state of covering the containers. All balance readings are reset to zero. Place the rhodium catalyst, phosphorus ligand, and toluene solution into the formylation reactor 1, deionized water into the extraction container 2, and the Raney nickel catalyst into the hydrogenation reactor 3. Confirm that all valves are closed, the containers are gasketed (i.e., the first gasket 14, the second gasket 15, and the third gasket 16) and are tightened and closed with bolts, the heating kettle jackets are in a standby state, and the readings of the first balance 12 and the second balance 13 are reset to zero.

[0044] (2) Nitrogen is passed through the formylation reactor 1 to verify the air tightness of the device. After verifying the air tightness, nitrogen replacement is performed, and the former air tightness verification pressure is maintained and stirring is started. After the pressure stabilizes, the liquid dissolved gas replacement is completed, and the first needle hole valve 17 is opened to vent and release the pressure, and then nitrogen replacement is performed twice (without stirring). The first needle hole valve 17 is closed to vent, and the nitrogen replacement is completed. The nitrogen source is switched to the synthesis gas source, and the synthesis gas replacement is performed in the same way.

[0045] (3) The synthesis gas is introduced into the formylation reactor 1. The heating and stirring device is adjusted to set the experimental temperature, pressure and time. When the reaction starts, the mass changes of the first level 12 and the second level 13 are recorded.

[0046] (4) After the reaction is completed, the kettle jacket is removed and cooled to room temperature, and nitrogen is replaced. Before the solution in the formylation reactor 1 that has completed the formylation reaction is introduced into the extraction container 2, it should be ensured that all pipelines are closed except for the pipeline between the bottom discharge valve of the formylation reactor 1 and the extraction container 2 and the venting pipeline of the extraction container 2. Specifically, the gas source and gas source pipeline valves of the formylation reactor 1 and the extraction container 2 are closed (i.e., the eleventh needle hole valve 34 and the twelfth needle hole valve 35 are closed), and the valve status is checked, wherein the first needle hole valve 17 and the fifth needle hole valve 22 are closed, the second needle hole valve 18 and the fourth needle hole valve 20 are opened, and the discharge valves of the formylation reactor 1 and the extraction container 2 are closed. Open the discharge valve of the formylation reactor 1, slowly open the gas source of the formylation reactor 1 and the valve of the gas source pipeline (i.e., the eleventh needle hole valve 34), and start the introduction. Observe the liquid level of extraction container 2. When the liquid level stops rising, close the gas source of formylation reactor 1 (i.e., the eleventh needle hole valve 34), close the discharge valve of formylation reactor 1, close the second needle hole valve 18, and the fourth needle hole valve 20. At this time, the solution is introduced into extraction container 2, and all branches of the two containers are closed.

[0047] (5) Starting the stirring of the extraction container 2 (i.e., the second rotor 10), and allowing the mixture to stand and separate into layers after the stirring is completed.

[0048] (6) Before the aqueous solution in the extraction container 2 is introduced into the hydrogenation reactor 3, in addition to ensuring that the aqueous solution enters the hydrogenation reactor 3 smoothly, it is also necessary to ensure that the water layer and the toluene layer are clearly separated and do not mix with each other. To achieve this purpose, the solution at the oil-water interface can be selected. Ensure that the gas source of the extraction container 2 and the hydrogenation reactor 3 and the gas source pipeline valve (the twelfth needle hole valve 35, the thirteenth needle hole valve 36) are closed, and check the valve status. Except for the pipeline connecting the discharge valve of the extraction container 2 and the hydrogenation reactor 3 and the venting pipeline of the hydrogenation reactor 3, the remaining branches are closed, specifically the second needle hole valve 18, the fourth needle hole valve 20, the fifth needle hole valve 22, and the sixth needle hole valve 23 are closed, the seventh needle hole valve 24 and the third needle hole valve 19 are opened, and the discharge valves of the two containers are closed. Open the discharge valve at the bottom of the extraction container 2, slowly open the gas source (needle hole valve 35), and observe the liquid level of the extraction container 2 to cut off the water and remove the oil-water mixture. When the liquid level approaches the oil-water boundary, close the discharge valve of the extraction container 2 to prevent the toluene solution from mixing into the hydrogenation reactor 3, close the seventh needle valve 24, and turn off the nitrogen gas source. Open the sixth needle valve 23 and the ninth needle valve 32, open the discharge valve, slowly open the nitrogen gas source, introduce the oil-water interface solution into the first waste liquid collection bucket 4 and observe the liquid level until the oil-water interface disappears, immediately close the discharge valve, gas source, the ninth needle valve 32, and the sixth needle valve 23 to prevent water from mixing into the toluene solution. The remaining toluene solution is re-introduced into the formylation reactor 1 for use or exported using the collection bucket pipeline as needed.

[0049] (7) Pass nitrogen through the hydrogenation reactor 3 to verify the air tightness of the device. After verifying the air tightness, perform nitrogen replacement, maintain the air tightness verification pressure and start stirring. After the pressure stabilizes, it means that the liquid dissolved gas replacement is completed. Open the third needle hole valve 19 to vent and release the pressure, then perform two replacements in the same way (without stirring), close the first needle hole valve 19 for venting, and the nitrogen replacement is completed. Cut off the nitrogen source and perform hydrogen replacement in the same way.

[0050] (8) Hydrogen is introduced into the hydrogenation reactor. The heating and stirring device is adjusted to set the experimental temperature, pressure and time. When the reaction starts, the mass changes of the first day level 12 and the second day level 13 are recorded.

[0051] (9) After the reaction is completed, remove the reactor jacket, cool it to room temperature, and replace it with nitrogen.

[0052] (10) Open the tenth needle hole valve 33 and the eighth needle hole valve 29, open the discharge valve of the hydrogenation reactor 3, slowly increase the pressure with nitrogen gas source until the liquid level is emptied, and then close all the above valves and gas sources.

[0053] The utility model connects three reactions into a set of devices and adopts a closed process, which reduces the risk of leakage and poisoning and improves safety. After the catalyst, solution, etc. are added, the whole process can be operated only by opening and closing the valve, which simplifies the operation steps. The problem that the quality change of synthesis gas and hydrogen consumption cannot be accurately measured due to factors such as solution wall adhesion is solved, and the experimental results are more accurate.

[0054] Although the functions and working processes of the utility model are described above in conjunction with the accompanying drawings, the utility model is not limited to the above-mentioned specific functions and working processes, and the above-mentioned specific implementation methods are merely illustrative rather than restrictive. Under the enlightenment of the utility model, ordinary technicians in this field can also make many forms without departing from the scope of protection of the purpose of the utility model and the claims, which are all within the protection of the utility model.

Claims

1. A reaction-extraction experimental device, comprising a formylation reactor (1), an extraction container (2), and a hydrogenation reactor (3), characterized in that: The discharge valve at the bottom of the formylation reactor (1) is connected to the top feed port of the extraction container (2) through a pipeline; the discharge valve at the bottom of the extraction container (2) is connected to the top feed port of the formylation reactor (1), the top feed port of the hydrogenation reactor (3), and the first waste liquid collection bucket (4) through pipelines; the discharge valve at the bottom of the hydrogenation reactor (3) is connected to the second waste liquid collection bucket (5) through a pipeline; the tops of the formylation reactor (1), the extraction container (2), and the hydrogenation reactor (3) are all provided with gas source pipelines and venting pipelines; the formylation reactor (1), the extraction container (2), and the hydrogenation reactor (3) are ... are connected to the first waste liquid collection bucket (4) through pipelines; the discharge valve at the bottom of the hydrogenation reactor (3) is connected to the second waste liquid collection bucket (5) through pipelines; the tops of the formylation reactor (1), the extraction container (2), and the hydrogenation reactor (3) are all provided with gas source pipelines and venting pipelines; the formylation reactor (1) The gas source pipelines at the top of the formylation reactor (1), the extraction container (2) and the hydrogenation reactor (3) are respectively provided with an eleventh needle hole valve (34), a twelfth needle hole valve (35) and a thirteenth needle hole valve (36); the venting pipelines at the top of the formylation reactor (1), the extraction container (2) and the hydrogenation reactor (3) are respectively provided with a first needle hole valve (17), a second needle hole valve (18) and a third needle hole valve (19); the bottoms of the formylation reactor (1) and the hydrogenation reactor (3) are respectively provided with a first balance (12) and a second balance (13).

2. The reaction-extraction experimental device according to claim 1, characterized in that: The formylation reaction kettle (1), the extraction container (2) and the hydrogenation reaction kettle (3) are respectively provided with a first kettle jacket (6), a second kettle jacket (7) and a third kettle jacket (8) which are detachable and integrated with stirring and heating, and are respectively provided with a first rotor (9), a second rotor (10) and a third rotor (11) for stirring; the formylation reaction kettle (1) and the hydrogenation reaction kettle (3) are both provided with brackets on the outside of the kettle bodies, and are respectively fixed to a first balance (12) and a second balance (13) through the brackets.

3. The reaction-extraction experimental device according to claim 1, characterized in that: The formylation reaction kettle (1) is composed of a stainless steel cylindrical body and a stainless steel cover. The bottom of the stainless steel cylindrical body is an arc bottom and is equipped with a discharge valve. A first polytetrafluoroethylene gasket (14) is arranged between the top of the stainless steel cylindrical body and the stainless steel cover and is fastened by bolts.

4. The reaction-extraction experimental device according to claim 1, characterized in that: The extraction container (2) is composed of a transparent glass cylindrical body and a glass cover. The bottom of the glass cylindrical body is an arc bottom and is equipped with a discharge valve. A third tetrafluoroethylene gasket (16) is arranged between the top of the glass cylindrical body and the glass cover and is fastened by bolts.

5. The reaction-extraction experimental device according to claim 1, characterized in that: The hydrogenation reactor (3) is composed of a stainless steel cylindrical body and a stainless steel cover. The bottom of the stainless steel cylindrical body is an arc bottom and is equipped with a discharge valve. A second tetrafluoro gasket (15) is arranged between the top of the stainless steel cylindrical body and the stainless steel cover and is fastened by bolts.

6. The reaction-extraction experimental device according to claim 1, characterized in that: A fourth needle hole valve (20) and a first clamping type vacuum quick release flange (21) are provided on the pipeline connecting the bottom discharge valve of the formylation reaction kettle (1) and the top feed port of the extraction container (2); the fourth needle hole valve (20) is located at one end of the extraction container (2), and the first clamping type vacuum quick release flange (21) is located at one end of the formylation reaction kettle (1).

7. The reaction-extraction experimental device according to claim 1, characterized in that: A fifth needle hole valve (22) and a second clamping type vacuum quick release flange (25) are provided on the pipeline connecting the bottom discharge valve of the extraction container (2) and the top feed port of the formylation reactor (1); a sixth needle hole valve (23) and a third clamping type vacuum quick release flange (26) are provided on the pipeline connecting the bottom discharge valve of the extraction container (2) and the first waste liquid collection bucket (4); and a seventh needle hole valve (24) and a fourth clamping type vacuum quick release flange (27) are provided on the pipeline connecting the bottom discharge valve of the extraction container (2) and the top feed port of the hydrogenation reactor (3).

8. The reaction-extraction experimental device according to claim 1, characterized in that: The first waste liquid collection barrel (4) and the second waste liquid collection barrel (5) are both provided with drain pipes. The drain pipe of the first waste liquid collection barrel (4) is provided with a ninth needle hole valve (32) and a sixth clamping type vacuum quick release flange (30), and the drain pipe of the second waste liquid collection barrel (5) is provided with a tenth needle hole valve (33) and a seventh clamping type vacuum quick release flange (31).

9. The reaction-extraction experimental device according to claim 1, characterized in that: A fifth clamping type vacuum quick release flange (28) and an eighth needle hole valve (29) are provided on the pipeline connecting the bottom discharge valve of the hydrogenation reactor (3) and the second waste liquid collection barrel (5); the fifth clamping type vacuum quick release flange (28) is located at one end of the hydrogenation reactor (3), and the eighth needle hole valve (29) is located at one end of the second waste liquid collection barrel (5).

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