Grignard reagent synthesis explosion-proof reaction kettle

Abstract

The application provides a Grignard reagent synthesis explosion-proof reaction kettle, and belongs to the technical field of explosion-proof reaction kettles. The Grignard reagent synthesis explosion-proof reaction kettle comprises an adsorption structure and a neutralization structure, the adsorption structure comprises a cooling assembly, an adsorption assembly, a fixed pipe and a safety valve arranged on one side of the reaction kettle. In the application, a pressure sensor is arranged in the reaction kettle to detect the pressure value inside the reaction kettle. When the detected pressure value is greater than the preset value of the controller, the controller starts the safety valve to release gas through the fixed pipe to reduce the pressure. The discharged gas is cooled in the cooling cavity, and the impurities and organic matters in the gas are adsorbed by the activated carbon in the adsorption cavity, so that the components harmful to the environment and the human body in the gas are reduced. The two sides in the storage tank store acidic and alkaline solutions respectively, and the acid and alkaline substances in the gas are neutralized. The gas treated by cooling, adsorption and neutralization is finally discharged, so that the health and environmental protection purposes are achieved.

Description

Technical Field

[0001] This application relates to the field of explosion-proof reactor technology, and more specifically, to an explosion-proof reactor for the synthesis of Grignard reagents. Background Technology

[0002] Grignard reagents are an extremely important class of reagents in organic chemistry and are core tools for constructing complex molecules. In the preparation of aminoethanol diphenylboronic acid ester, Grignard reagents play a key role. Their application is mainly based on their strong nucleophilicity and carbon-carbon bond forming ability. Aminoethanol diphenylboronic acid ester usually contains phenyl, borate ester and aminoethanol structural fragments. Grignard reagents can react with compounds containing borate ester precursors or related intermediates to introduce organic groups such as phenyl through nucleophilic attack and construct the carbon skeleton of the target molecule.

[0003] Grignard reagent synthesis is usually an exothermic reaction. During the synthesis process, if the rate of exothermic reaction exceeds the rate of heat removal, the temperature of the system inside the reactor will rise sharply. This may lead to thermal runaway, as well as gas expansion or solvent evaporation, which in turn will increase the pressure inside the reactor and pose a risk of explosion. Therefore, reactors are usually equipped with safety valves. However, the gas discharged through the safety valve contains a large number of harmful substances. If the gas is discharged directly, it will not only cause the loss of raw materials, but also harm the environment and the health of people in the surrounding area. Utility Model Content

[0004] To overcome the above deficiencies, this application provides an explosion-proof reaction vessel for the synthesis of Grignard reagents, which aims to improve the problem that the gas discharged from the safety valve contains a large number of harmful substances. If the gas is discharged directly, it will not only cause the loss of raw materials, but also harm the environment and the health of people in the surrounding area.

[0005] This application provides an explosion-proof reaction vessel for synthesizing Grignard reagents, including an adsorption structure and a neutralization structure. The adsorption structure includes a cooling component, an adsorption component, a fixed tube, and a safety valve disposed on one side of the reaction vessel. The adsorption component is fixedly connected to the bottom of the cooling component. The fixed tube is fixedly connected to one side of the reaction vessel, and its bottom is fixedly connected to the top of the cooling component. The safety valve is disposed on the surface of the fixed tube, and the input end of the safety valve is connected to the output end of a pressure sensor installed inside the reaction vessel. The neutralization structure includes a storage tank, a connecting tube, a partition plate, and a liquid infusion fitting. The storage tank is located on one side of the cooling component. The connecting tube is fixedly connected to the back of the storage tank. The partition plate is fixedly connected to the center of the inner cavity of the storage tank. The liquid infusion fitting is disposed on the surface of the storage tank.

[0006] In one specific implementation, the cooling assembly includes a cooling cavity, a coolant pipe, and a support plate. The cooling cavity is fixedly connected to the surface of the reactor via a support frame. The coolant pipe is disposed in the inner cavity of the cooling cavity. The support plate is located on the surface of the coolant pipe, and one side of the support plate is fixedly connected to the inner wall of the cooling assembly.

[0007] In the above process, the cooling chamber is used to provide a closed cooling space for the gas, the support plate is used to support the coolant pipe to improve its stability, and the coolant pipe is used to transport coolant in order to cool the discharged gas.

[0008] In one specific embodiment, the adsorption assembly includes an adsorption chamber and a sealing plate, the adsorption chamber being fixedly connected to the bottom of the cooling chamber, and the sealing plate being located at the bottom of the adsorption chamber.

[0009] In the above process, the adsorption chamber provides space for the gas to be adsorbed by activated carbon, and the sealing plate is used to seal the bottom of the adsorption chamber to prevent gas leakage.

[0010] In one specific embodiment, the adsorption assembly further includes a placement box and a support net. The placement box is fixedly connected to the bottom of the sealing plate and is detachably connected to the inner cavity of the adsorption chamber. The support net is fixedly connected to the inner cavity of the placement box.

[0011] In the above process, the placement box and the support net work together to place the activated carbon, while the support net allows the gas to circulate.

[0012] In one specific embodiment, the adsorption assembly further includes a fixing frame and a bellows. The fixing frame is located at the bottom of the sealing plate and one side of it is fixedly connected to the surface of the reactor. The end of the connecting pipe away from the storage tank passes through the fixing frame and is fixedly connected to the bottom of the bellows. The bellows is fixedly connected to the bottom of the sealing plate, and the bottom of the bellows is fixedly connected to the fixing frame.

[0013] In the above implementation process, the fixing frame is used to support the top component, and the bellows can extend and retract vertically, so that the height of the sealing plate can be adjusted to allow for the addition or replacement of activated carbon.

[0014] In one specific embodiment, the adsorption assembly further includes a compression spring that provides support for the sealing plate, the compression spring being sleeved on the surface of the bellows, and its top and bottom being fixedly connected to the bottom of the sealing plate and the top of the fixing frame, respectively.

[0015] In the above process, the compression spring is a stainless steel spring and is always in a compressed state, providing an upward supporting force for the sealing plate, so that the sealing plate can be tightly attached to the bottom of the adsorption cavity.

[0016] In one specific embodiment, the adsorption assembly further includes a sealing ring for sealing the gap between the sealing plate and the adsorption chamber, the sealing ring being fixedly connected to the top of the sealing plate and having its top fitting against the bottom of the adsorption chamber.

[0017] In the above process, the sealing ring is used to seal the space between the sealing plate and the bottom of the adsorption chamber, thereby preventing gas leakage.

[0018] In one specific implementation, the infusion tubing includes a first catheter and a second catheter. The first catheter is fixedly connected to the left side of the inner cavity of the storage box, and its rear end is fixedly connected to a connecting pipe. The second catheter is fixedly connected to the right side of the partition plate.

[0019] In the above process, the interior of the storage box is divided by a partition plate, with an acidic solution stored on the left and an alkaline solution stored on the right. The first conduit delivers the gas to the solution on the left to neutralize the alkaline components in the gas, and then the second conduit delivers the gas to the solution on the right to neutralize the acidic substances in the solution, thereby removing the acidic and alkaline components from the gas.

[0020] In one specific embodiment, the infusion fitting further includes a discharge pipe for discharging gas from inside the storage tank, the discharge pipe being fixedly connected to the right side of the storage tank.

[0021] In the above process, the discharge pipe is used to discharge the treated gas from the inside of the storage tank. It can be connected to an external storage tank so that some components of the gas can be recycled.

[0022] In one specific implementation, the infusion tubing further includes four cap assemblies, which are respectively fixedly connected to the front and top sides of the storage tank, and their surfaces are threaded to a sealing cap. The top and front cap assemblies are used to add liquid to the inside of the storage tank.

[0023] In the above implementation process, the two upper pipe cap assemblies are used to add acid and alkaline solutions to the inside of the storage box, respectively, and the two lower pipe cap assemblies are used to drain the acid and alkaline solutions from the inside of the storage box.

[0024] Compared with the prior art, the beneficial effects of this application are as follows: A pressure sensor is installed inside the reactor to detect the internal pressure value. When the detected pressure value is greater than the preset value of the controller, the controller activates the safety valve to release gas and reduce pressure through the fixed pipe. The discharged gas is cooled by the cooling chamber and impurities and organic matter are adsorbed by activated carbon inside the adsorption chamber, reducing the components in the gas that are harmful to the environment and human body. Then the gas is transported to the inside of the storage tank. Acidic and alkaline solutions are stored on both sides of the storage tank to neutralize the acidic and alkaline substances in the gas. The gas that has been cooled, adsorbed and neutralized is finally discharged, thereby achieving the purpose of health and environmental protection. Attached Figure Description

[0025] To more clearly illustrate the technical solutions of the embodiments of this application, the drawings used in the embodiments will be briefly introduced below. It should be understood that the following drawings only show some embodiments of this application and should not be regarded as a limitation of the scope. For those skilled in the art, other related drawings can be obtained from these drawings without creative effort.

[0026] Figure 1 This is a schematic diagram of an explosion-proof reaction vessel for synthesizing Grignard reagents provided in an embodiment of this application;

[0027] Figure 2 A schematic diagram of the connection structure of a cooling assembly, an adsorption assembly, and a fixing tube for an explosion-proof reactor for the synthesis of Grignard reagents provided in this application;

[0028] Figure 3 A cross-sectional structural diagram of the cooling cavity provided in the embodiments of this application;

[0029] Figure 4 This is a schematic diagram of the front view structure of the adsorption cavity provided in the embodiments of this application;

[0030] Figure 5 A schematic diagram of the connection structure of the sealing plate, the placement box, and the support mesh provided in the embodiments of this application;

[0031] Figure 6 A cross-sectional view of the storage box provided in an embodiment of this application;

[0032] Figure 7 A cross-sectional structural diagram of the storage box provided for an embodiment of this application;

[0033] Figure 8 Provided for the implementation of this application Figure 3 A magnified view of a portion of point A in the middle.

[0034] In the diagram: 10, Adsorption structure; 110, Cooling assembly; 1101, Coolant pipe; 1102, Support plate; 120, Adsorption assembly; 1201, Sealing plate; 1202, Placement box; 1203, Support mesh; 1204, Fixing frame; 1205, Corrugated pipe; 1206, Compression spring; 1207, Sealing ring; 130, Fixing pipe; 140, Safety valve; 20, Neutralization structure; 210, Storage tank; 220, Connecting pipe; 230, Divider plate; 240, Infusion fittings; 2401, First conduit; 2402, Second conduit; 2403, Discharge pipe; 2404, Pipe cap assembly. Detailed Implementation

[0035] The technical solutions in the embodiments of this application will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of this application, and not all embodiments.

[0036] Please see Figure 1 This application provides an explosion-proof reaction vessel for synthesizing Grignard reagents, including an adsorption structure 10 and a neutralization structure 20.

[0037] Please see Figure 1 and Figure 2 The adsorption structure 10 includes a cooling component 110, an adsorption component 120, a fixed tube 130, and a safety valve 140, all disposed on one side of the reactor. The adsorption component 120 is fixedly connected to the bottom of the cooling component 110. The fixed tube 130 is fixedly connected to one side of the reactor, and its bottom is fixedly connected to the top of the cooling component 110. The safety valve 140 is disposed on the surface of the fixed tube 130, and the input end of the safety valve 140 is connected to the output end of a pressure sensor installed inside the reactor.

[0038] Please see Figure 2 and Figure 6 The neutralization structure 20 includes a storage tank 210, a connecting pipe 220, a partition plate 230, and an infusion fitting 240. The storage tank 210 is located on one side of the cooling assembly 110. The connecting pipe 220 is fixedly connected to the back of the storage tank 210. The partition plate 230 is fixedly connected to the center of the inner cavity of the storage tank 210. The infusion fitting 240 is disposed on the surface of the storage tank 210.

[0039] In a specific configuration, the cooling assembly 110 includes a cooling chamber, a coolant pipe 1101, and a support plate 1102. The cooling chamber is fixedly connected to the surface of the reactor via a support frame. The coolant pipe 1101 is disposed in the inner cavity of the cooling chamber. The support plate 1102 is located on the surface of the coolant pipe 1101, and one side of the support plate 1102 is fixedly connected to the inner wall of the cooling assembly 110. The cooling chamber is used to provide a sealed cooling space for the gas. The support plate 1102 is used to support the coolant pipe 1101 and improve its stability. The coolant pipe 1101 is used to transport coolant in order to cool the discharged gas.

[0040] In a specific configuration, the adsorption assembly 120 includes an adsorption chamber and a sealing plate 1201. The adsorption chamber is fixedly connected to the bottom of the cooling chamber, and the sealing plate 1201 is located at the bottom of the adsorption chamber. The adsorption chamber provides space for the gas to be adsorbed by activated carbon, and the sealing plate 1201 is used to seal the bottom of the adsorption chamber to prevent gas leakage.

[0041] In a specific configuration, the adsorption assembly 120 also includes a placement box 1202 and a support net 1203. The placement box 1202 is fixedly connected to the bottom of the sealing plate 1201, and the placement box 1202 is detachably connected to the inner cavity of the adsorption chamber. The support net 1203 is fixedly connected to the inner cavity of the placement box 1202. The placement box 1202 and the support net 1203 work together to place activated carbon, and the gas can circulate under the action of the support net 1203.

[0042] In a specific configuration, the adsorption assembly 120 also includes a fixing frame 1204 and a bellows 1205. The fixing frame 1204 is located at the bottom of the sealing plate 1201, and one side of it is fixedly connected to the surface of the reactor. The end of the connecting pipe 220 away from the storage tank 210 passes through the fixing frame 1204 and is fixedly connected to the bottom of the bellows 1205. The bellows 1205 is fixedly connected to the bottom of the sealing plate 1201, and the bottom of the bellows 1205 is fixedly connected to the fixing frame 1204. The fixing frame 1204 is used to support the top components. The bellows 1205 can extend and retract vertically, thereby allowing the height of the sealing plate 1201 to be adjusted for adding or replacing activated carbon.

[0043] In a specific configuration, the adsorption assembly 120 also includes a compression spring 1206 that provides support for the sealing plate 1201. The compression spring 1206 is sleeved on the surface of the bellows 1205, and its top and bottom are fixedly connected to the bottom of the sealing plate 1201 and the top of the fixing frame 1204, respectively. The compression spring 1206 is a stainless steel spring and is always in a compressed state, providing an upward support force for the sealing plate 1201, so that the sealing plate 1201 can be tightly attached to the bottom of the adsorption cavity.

[0044] In a specific configuration, the adsorption assembly 120 also includes a sealing ring 1207 for sealing the gap between the sealing plate 1201 and the adsorption chamber. The sealing ring 1207 is fixedly connected to the top of the sealing plate 1201, and its top is in contact with the bottom of the adsorption chamber. The sealing ring 1207 is used to seal the space between the sealing plate 1201 and the bottom of the adsorption chamber, thereby preventing gas leakage.

[0045] In a specific configuration, the infusion tubing 240 includes a first conduit 2401 and a second conduit 2402. The first conduit 2401 is fixedly connected to the left side of the inner cavity of the storage tank 210, and its rear end is fixedly connected to the connecting pipe 220. The second conduit 2402 is fixedly connected to the right side of the partition plate 230. After being separated by the partition plate 230, the storage tank 210 stores an acidic solution on the left and an alkaline solution on the right. The first conduit 2401 delivers the gas to the solution on the left to neutralize the alkaline components in the gas, and then the second conduit 2402 delivers the gas to the solution on the right to neutralize the acidic substances in the solution, thereby removing the acidic and alkaline components from the gas.

[0046] In a specific configuration, the infusion fitting 240 also includes a discharge pipe 2403 for discharging gas from inside the storage tank 210. The discharge pipe 2403 is fixedly connected to the right side of the storage tank 210. The discharge pipe 2403 is used to discharge the processed gas from inside the storage tank 210. It can be connected to an external storage tank so that some components in the gas can be recycled.

[0047] In a specific configuration, the infusion tubing 240 also includes four tube cap assemblies 2404. The four tube cap assemblies 2404 are fixedly connected to the front and top sides of the storage tank 210, and their surfaces are threaded to the sealing caps. The top and front sets of tube cap assemblies 2404 are used to add liquid to the inside of the storage tank 210, respectively. The two upper tube cap assemblies 2404 are used to add acid and alkaline solutions to the inside of the storage tank 210, respectively, and the two lower tube cap assemblies 2404 are used to drain the acid and alkaline solutions from the inside of the storage tank 210, respectively.

[0048] The working principle of the explosion-proof reactor for the synthesis of Grignard reagents is as follows: A pressure sensor is installed inside the reactor to detect the internal pressure value. When the detected pressure value is greater than the preset value of the controller, the controller activates the safety valve 140 to release and reduce the pressure through the fixed pipe 130. Cooling liquid circulates in the cooling liquid pipe 1101 to cool the discharged gas. Activated carbon is placed in the placement box 1202 to adsorb organic matter and impurities in the gas. The adsorbed gas is transported to the interior of the storage tank 210 through the connecting pipe 220. Acidic and alkaline solutions are stored on both sides inside the storage tank 210 to neutralize the alkaline and acidic components in the gas. Finally, the gas is discharged or collected through the discharge pipe 2403.

[0049] The above are merely specific embodiments of this application, but the scope of protection of this application is not limited thereto. Any variations or substitutions that can be easily conceived by those skilled in the art within the scope of the technology disclosed in this application should be included within the scope of protection of this application. Therefore, the scope of protection of this application should be determined by the scope of the claims.

Claims

1. An explosion-proof reaction vessel for synthesizing Grignard reagents, characterized in that, include The adsorption structure (10) includes a cooling component (110), an adsorption component (120), a fixed tube (130), and a safety valve (140) disposed on one side of the reactor. The adsorption component (120) is fixedly connected to the bottom of the cooling component (110). The fixed tube (130) is fixedly connected to one side of the reactor, and its bottom is fixedly connected to the top of the cooling component (110). The safety valve (140) is disposed on the surface of the fixed tube (130), and the input end of the safety valve (140) is connected to the output end of a pressure sensor installed inside the reactor. The neutralization structure (20) includes a storage tank (210), a connecting pipe (220), a partition plate (230), and an infusion fitting (240). The storage tank (210) is located on one side of the cooling assembly (110). The connecting pipe (220) is fixedly connected to the back of the storage tank (210). The partition plate (230) is fixedly connected to the center of the inner cavity of the storage tank (210). The infusion fitting (240) is disposed on the surface of the storage tank (210).

2. The explosion-proof reaction vessel for synthesizing Grignard reagents according to claim 1, characterized in that, The cooling assembly (110) includes a cooling chamber, a coolant pipe (1101), and a support plate (1102). The cooling chamber is fixedly connected to the surface of the reactor via a support frame. The coolant pipe (1101) is located in the inner cavity of the cooling chamber. The support plate (1102) is located on the surface of the coolant pipe (1101), and one side of the support plate (1102) is fixedly connected to the inner wall of the cooling assembly (110).

3. The explosion-proof reaction vessel for synthesizing Grignard reagents according to claim 1, characterized in that, The adsorption assembly (120) includes an adsorption chamber and a sealing plate (1201). The adsorption chamber is fixedly connected to the bottom of the cooling chamber, and the sealing plate (1201) is located at the bottom of the adsorption chamber.

4. The explosion-proof reaction vessel for synthesizing Grignard reagents according to claim 3, characterized in that, The adsorption assembly (120) further includes a placement box (1202) and a support net (1203). The placement box (1202) is fixedly connected to the bottom of the sealing plate (1201), and the placement box (1202) is detachably connected to the inner cavity of the adsorption chamber. The support net (1203) is fixedly connected to the inner cavity of the placement box (1202).

5. The explosion-proof reaction vessel for synthesizing Grignard reagents according to claim 3, characterized in that, The adsorption assembly (120) also includes a fixing frame (1204) and a bellows (1205). The fixing frame (1204) is located at the bottom of the sealing plate (1201) and one side of it is fixedly connected to the surface of the reactor. The end of the connecting pipe (220) away from the storage tank (210) passes through the fixing frame (1204) and is fixedly connected to the bottom of the bellows (1205). The bellows (1205) is fixedly connected to the bottom of the sealing plate (1201), and the bottom of the bellows (1205) is fixedly connected to the fixing frame (1204).

6. The explosion-proof reaction vessel for synthesizing Grignard reagents according to claim 5, characterized in that, The adsorption assembly (120) also includes a compression spring (1206) that provides support for the sealing plate (1201). The compression spring (1206) is sleeved on the surface of the bellows (1205), and its top and bottom are fixedly connected to the bottom of the sealing plate (1201) and the top of the fixing frame (1204), respectively.

7. The explosion-proof reaction vessel for synthesizing Grignard reagents according to claim 3, characterized in that, The adsorption assembly (120) further includes a sealing ring (1207) for sealing the gap between the sealing plate (1201) and the adsorption chamber. The sealing ring (1207) is fixedly connected to the top of the sealing plate (1201), and its top is in contact with the bottom of the adsorption chamber.

8. The explosion-proof reaction vessel for synthesizing Grignard reagents according to claim 1, characterized in that, The infusion fitting (240) includes a first catheter (2401) and a second catheter (2402). The first catheter (2401) is fixedly connected to the left side of the inner cavity of the storage box (210), and its rear end is fixedly connected to the connecting pipe (220). The second catheter (2402) is fixedly connected to the right side of the partition plate (230).

9. The explosion-proof reaction vessel for synthesizing Grignard reagents according to claim 1, characterized in that, The infusion fitting (240) also includes a discharge pipe (2403) for discharging gas from inside the storage tank (210), the discharge pipe (2403) being fixedly connected to the right side of the storage tank (210).

10. The explosion-proof reaction vessel for synthesizing Grignard reagents according to claim 1, characterized in that, The infusion tubing (240) also includes four cap assemblies (2404), which are fixedly connected to the front and top sides of the storage tank (210) respectively, and their surfaces are threaded to the sealing cap. The top and front cap assemblies (2404) are used to add liquid to the inside of the storage tank (210) respectively.

Images