Reaction kettle

Abstract

The utility model relates to a reaction kettle. The reaction kettle comprises a kettle cavity, a pressure controller and a first high-pressure gas source, the pressure controller comprises a thin pipe, one end of the thin pipe is an open end, the other end of the thin pipe is a closed end, the open end of the thin pipe is communicated with the kettle cavity, a sliding plug is arranged in a pipe cavity of the thin pipe, and the sliding plug is connected with the kettle cavity. The reaction kettle disclosed by the utility model can be simply and effectively used for continuously filling high-pressure gas raw materials into the reaction kettle, so that the gas raw materials are kept at the required high air pressure to carry out gas-liquid phase reaction, and the safety problem caused by overhigh air pressure of the kettle cavity is avoided.

Description

Technical Field

[0001] The utility model relates to the field of chemical industry, in particular to a reaction kettle. Background Art

[0002] Reactor is a commonly used chemical synthesis reaction equipment. In chemical synthesis reactions, many synthesis reactions are gas-liquid phase reactions. For gas-liquid phase reactions, high-pressure gas raw materials are usually required to achieve the reaction of gas raw materials with reactants in the liquid phase. For example, iopamidol is an iodinated X-ray contrast agent used for myelography, urography, angiography or CT enhanced scanning, etc. In the existing commonly used iopamidol synthesis reaction, reducing the iopamidol ester exchange product to the iopamidol reduction product is an important step in the iopamidol synthesis route. The commonly used synthesis method for reducing the iopamidol ester exchange product to the iopamidol reduction product is as follows: gas-liquid phase reaction:

[0003]

[0004] In the reactor, the pressure of the H2 raw material needs to be maintained at 9-11 atmospheres so that it can react with the iopamidol ester exchange product in the water solvent medium to generate the iopamidol reduced product.

[0005] For a reactor containing a high-pressure gas raw material for a gas-liquid phase reaction, the consumption of the gas raw material will cause the gas pressure of the gas raw material to decrease. Therefore, the reactor needs to be continuously filled with high-pressure gas raw material to keep the gas raw material at the required high pressure for continuous reaction. In addition, for a reactor containing a high-pressure gas raw material for a reaction, many abnormal factors (such as abnormal reactor heater causing the reactor cavity temperature to be too high, etc.) can easily cause the reactor cavity pressure to be too high, thereby causing safety problems. Therefore, for a reactor containing a high-pressure gas raw material for a gas-liquid phase reaction, it is very important for chemical synthesis to avoid excessive pressure in the reactor cavity. However, for a gas-liquid phase reaction that requires a high-pressure gas raw material, the structure of the existing reactor is difficult to simply and effectively use to realize the continuous filling of the reactor with high-pressure gas raw material to keep the gas raw material at the required high pressure for a gas-liquid phase reaction and to avoid safety problems caused by excessive pressure in the reactor cavity.

[0006] Therefore, there is a need in the art to develop a reactor that can be simply and effectively used to continuously fill the reactor with high-pressure gas raw materials so that the gas raw materials are maintained at the required high pressure for gas-liquid phase reaction and avoid safety problems caused by excessive gas pressure in the reactor chamber. Utility Model Content

[0007] The utility model aims to provide a reactor, which can be simply and effectively used to realize continuous filling of the reactor with high-pressure gas raw materials so that the gas raw materials are kept at a required high gas pressure for gas-liquid phase reaction and avoid safety problems caused by excessive gas pressure in the reactor cavity.

[0008] In a first aspect, the utility model provides a reaction kettle, the reaction kettle comprising a kettle chamber 1, a pressure controller and a first high-pressure gas source 2;

[0009] The pressure controller comprises a capillary tube 3, one end of which is an open end, and the other end of which is a closed end. The open end of the capillary tube is communicated with the kettle cavity. A sliding plug 4 is provided in the cavity of the capillary tube. The sliding plug is sealed with the inner wall of the cavity of the capillary tube. One end of the sliding plug is connected to the inner wall of the closed end of the capillary tube through a reset spring 5. A horizontal channel 6 is provided inside the sliding plug. A first through hole 7, a second through hole 8 and a third through hole 9 are provided on the wall of the capillary tube. The first through hole and the second through hole are located above the third through hole, and the first through hole and the second through hole are located on the same horizontal plane.

[0010] The first through hole is connected to the kettle chamber through a first gas pipe 10, the second through hole is connected to the first high-pressure gas source through a second gas pipe 11, the third through hole is connected to a third gas pipe 12, and a valve 13 is provided on the second gas pipe;

[0011] When the kettle chamber is connected to the outside atmosphere, the sliding plug blocks the first through hole and the second through hole, the horizontal channel inside the sliding plug is located below the first through hole and the second through hole, and the vertical distance between the horizontal channel inside the sliding plug and the first through hole is smaller than the vertical distance between the bottom outer wall of the sliding plug and the third through hole.

[0012] Preferably, the increased gas pressure in the kettle chamber causes the sliding plug to slide upward along the inner wall of the tube cavity of the capillary tube.

[0013] Preferably, the air pressure in the kettle chamber decreases so that the sliding plug slides downward along the inner wall of the tube cavity of the capillary tube.

[0014] Preferably, the reactor comprises a reactor for gas-liquid phase reaction.

[0015] Preferably, the gas-liquid phase reaction comprises a reaction of reducing the iopamidol transester to an iopamidol reduced product, and the reaction comprises:

[0016]

[0017] The iopamidol ester exchange product in the water solvent is reduced to the iopamidol reduced product using 9-11 atmospheres of H2, thereby obtaining the iopamidol reduced product.

[0018] Preferably, the first high-pressure gas source comprises a first high-pressure hydrogen source.

[0019] Preferably, the gas pressure of the first high-pressure gas source is 9-11 atmospheres (such as 9, 10 or 11 atmospheres).

[0020] Preferably, the kettle cavity contains water and iopamidol ester exchange product.

[0021] Preferably, when the gas pressure of the kettle chamber is 9-11 atmospheres (such as 9, 10 or 11 atmospheres), the horizontal channel inside the sliding plug is communicated with the first through hole and the second through hole.

[0022] Preferably, when the gas pressure in the kettle chamber is greater than 11-13 atmospheres (such as greater than 11, 12 or 13 atmospheres), the lumen of the capillary tube below the bottom of the sliding plug is in communication with the third through hole.

[0023] Preferably, the reactor further comprises a second high-pressure gas source.

[0024] Preferably, the second high-pressure gas source is connected to the kettle chamber through a fourth gas pipe.

[0025] Preferably, the fourth gas pipe is provided with a valve.

[0026] Preferably, the second high-pressure gas source comprises a second high-pressure hydrogen source.

[0027] Preferably, the gas pressure of the second high-pressure gas source is 10-11.5 atmospheres (such as 10, 11 or 11.5 atmospheres).

[0028] Preferably, when the kettle cavity is connected to the outside atmosphere, the vertical distance between the horizontal channel inside the sliding plug and the center of the first through hole is smaller than the vertical distance between the bottom outer wall of the sliding plug and the center of the third through hole.

[0029] Preferably, when the kettle cavity is connected to the outside atmosphere, the vertical distance between the channel axis of the horizontal channel inside the sliding plug and the center of the first through hole is smaller than the vertical distance between the bottom outer wall of the sliding plug and the center of the third through hole.

[0030] Preferably, when the kettle cavity is communicated with the outside atmosphere, the horizontal channel inside the sliding plug is located above the third through hole.

[0031] Preferably, when the kettle cavity is communicated with the outside atmosphere, the bottom outer wall of the sliding plug is located below the third through hole.

[0032] Preferably, the reactor further comprises a sampler, which comprises a material taking tube 14 and a sampling bottle 15, one end of the material taking tube is communicated with the reactor cavity, and the other end of the material taking tube is a closed end, a valve 13 is provided on the material taking tube, and the sampling bottle is connected to the material taking tube.

[0033] Preferably, a liquid pump is provided on the material taking pipe.

[0034] Preferably, the material taking pipe is connected to a third high-pressure gas source 17 via a fifth gas pipe 16 , and a valve 13 is provided on the fifth gas pipe.

[0035] Preferably, the third high-pressure gas source includes a third high-pressure hydrogen source or a third high-pressure nitrogen source.

[0036] Preferably, the third high-pressure gas source is used to inflate and clear the material extraction pipe.

[0037] Preferably, the gas pressure of the third high-pressure gas source is 11.5 atmospheres.

[0038] Preferably, one end of the fifth gas pipe is connected to the closed end of the material extraction pipe.

[0039] Preferably, the valve on the material taking pipe is located between a connection point between one end of the material taking pipe and the kettle chamber and a connection point between the sampling bottle and the material taking pipe.

[0040] Preferably, one end of the material taking pipe is inserted into the bottom of the kettle cavity.

[0041] Preferably, the capillary comprises a cylindrical tube.

[0042] Preferably, the open end of the capillary is connected to the cavity wall of the kettle cavity.

[0043] Preferably, the capillary is a transparent capillary.

[0044] Preferably, the side wall of the capillary is provided with scale lines.

[0045] Preferably, the scale line can quantitatively indicate the gas pressure in the kettle chamber.

[0046] Preferably, the gas pressure in the kettle chamber is quantitatively indicated by the position of the bottom outer wall of the sliding plug corresponding to the scale line.

[0047] Preferably, the first gas tube is a transparent tube.

[0048] Preferably, the second gas tube is a transparent tube.

[0049] Preferably, the third gas tube is a transparent tube.

[0050] Preferably, the centers of the first through hole and the second through hole are located on the same horizontal plane.

[0051] Preferably, the first through hole and the second through hole are both circular holes.

[0052] Preferably, the first through hole and the second through hole have the same hole size.

[0053] Preferably, the first through hole and the second through hole are the same hole.

[0054] Preferably, the horizontal channel inside the sliding plug is a cylindrical channel.

[0055] Preferably, the sliding plug is a cylindrical sliding plug.

[0056] Preferably, the sliding plug can slide along the inner wall of the lumen of the thin tube.

[0057] Preferably, the sliding plug can slide freely along the inner wall of the lumen of the capillary tube.

[0058] Preferably, the channel opening of the horizontal channel inside the sliding plug is a circular channel opening.

[0059] Preferably, the channel opening of the horizontal channel inside the sliding plug has the same size as the first through hole and the second through hole.

[0060] Preferably, the channel opening of the horizontal channel inside the sliding plug is the same as the holes of the first through hole and the second through hole.

[0061] Preferably, a pipe opening at one end of the first gas pipe is connected to the first through hole, a pipe opening at the other end of the first gas pipe is connected to the cavity wall of the kettle cavity, and the first gas pipe is in communication with the kettle cavity.

[0062] Preferably, the first gas pipe is located outside the outer wall of the capillary tube.

[0063] Preferably, the first gas pipe is located outside the outer wall of the kettle chamber and the outer wall of the capillary tube.

[0064] Preferably, the second gas pipe is located outside the outer wall of the capillary tube.

[0065] Preferably, the third gas pipe is located outside the outer wall of the capillary tube.

[0066] Preferably, the third gas pipe is provided with an exhaust gas collector or processor.

[0067] Preferably, the third gas pipe is provided with a hydrogen collection or processing device.

[0068] Preferably, one end of the sliding plug is vertically connected to the inner wall of the closed end of the capillary tube via a return spring.

[0069] Preferably, the reactor further comprises a stirrer.

[0070] Preferably, the stirrer is capable of stirring the kettle cavity.

[0071] Preferably, the reactor further comprises a heater.

[0072] Preferably, the heater is capable of heating the kettle cavity.

[0073] Preferably, the reactor further comprises a gas release valve.

[0074] Preferably, the air release valve is capable of releasing air from the kettle chamber.

[0075] Preferably, the connection or connection includes communication.

[0076] Preferably, the connection or connection is a fixed connection or a detachable connection.

[0077] In a second aspect, the present invention provides a method for preparing an iopamidol reduction product by using the reactor as described in the first aspect of the present invention, wherein the method comprises:

[0078]

[0079] The iopamidol ester exchange product in the water solvent is reduced to the iopamidol reduced product using H2, thereby obtaining the iopamidol reduced product.

[0080] Preferably, the gas pressure of the H2 raw material is 9-11 atmospheres (such as 9, 10 or 11 atmospheres).

[0081] Preferably, the first high-pressure gas source comprises a first high-pressure hydrogen source.

[0082] Preferably, the gas pressure of the first high-pressure gas source is 9-11 atmospheres (such as 9, 10 or 11 atmospheres).

[0083] Preferably, the kettle cavity contains water and iopamidol ester exchange product.

[0084] Preferably, when the gas pressure of the kettle chamber is 9-11 atmospheres (such as 9, 10 or 11 atmospheres), the horizontal channel inside the sliding plug is communicated with the first through hole and the second through hole.

[0085] Preferably, when the gas pressure in the kettle chamber is greater than 11-13 atmospheres (such as greater than 11, 12 or 13 atmospheres), the lumen of the capillary tube below the bottom of the sliding plug is in communication with the third through hole.

[0086] Preferably, the second high-pressure gas source comprises a second high-pressure hydrogen source.

[0087] Preferably, the gas pressure of the second high-pressure gas source is 10-11.5 atmospheres (such as 10, 11 or 11.5 atmospheres).

[0088] Preferably, the method comprises:

[0089] (1) When the horizontal channel inside the sliding plug is connected to the first through hole and the second through hole, the H2 gas pressure in the reactor chamber is 10 atmospheres;

[0090] (2) The first high-pressure gas source contains H2 raw material at 10 atmospheres, the valve on the second gas pipe is closed, and the H2 raw material at 11 atmospheres is first filled into the kettle cavity, and then the H2 filling is stopped. At this time, the horizontal channel inside the sliding plug is located above the first through hole and the second through hole, and the valve on the second gas pipe is opened. As the H2 raw material in the reactor is continuously reacted and consumed, the H2 pressure in the kettle cavity is continuously reduced, and the sliding plug slides downward along the inner wall of the tube cavity of the capillary. When the H2 pressure in the kettle cavity drops to 10 atmospheres, the horizontal channel inside the sliding plug is communicated with the first through hole and the second through hole. At this time, the H2 raw material from the first high-pressure gas source is filled into the kettle cavity through the second gas pipe, the horizontal channel inside the sliding plug and the second gas pipe. The H2 raw material at 10 atmospheres is ensured to be kept at 10 atmospheres, so that the H2 reacts with the iopamidol ester exchange product in the water solvent to generate the iopamidol reduced product, thereby preparing the iopamidol reduced product.

[0091] Preferably, in the step (1), when the H2 gas pressure in the kettle chamber is 12 atmospheres, the lumen of the capillary tube below the bottom of the sliding plug is in communication with the third through hole.

[0092] Preferably, in the step (1), the weight of the return spring and the sliding plug is adjusted to achieve a H2 gas pressure of 10 atmospheres in the kettle chamber when the horizontal channel inside the sliding plug is connected to the first through hole and the second through hole.

[0093] Preferably, in step (1), by adjusting the weight of the return spring and the sliding plug, when the H2 gas pressure in the kettle chamber is 12 atmospheres, the lumen of the capillary tube below the bottom of the sliding plug is connected to the third through hole.

[0094] Preferably, the adjusting the return spring includes adjusting the elastic coefficient and stiffness of the return spring.

[0095] Preferably, in the step (2), H2 raw material at 11 atmospheres of pressure is first charged into the reactor chamber through another high-pressure H2 source and then the charging of H2 is stopped.

[0096] Preferably, in the step (2), the reactor chamber is first charged with H2 raw material at 11 atmospheres through a second high-pressure gas source containing H2 raw material at 11 atmospheres, and then the charging of H2 is stopped.

[0097] Preferably, in step (2), during the reaction process, if abnormal factors occur that cause the air pressure in the kettle chamber to continue to increase, the sliding plug slides upward along the inner wall of the lumen of the capillary tube, and when the air pressure in the kettle chamber rises to 12 atmospheres, at this time, the lumen of the capillary tube below the bottom of the sliding plug is connected to the third through hole, and the high-pressure gas in the kettle chamber will be discharged in time through the third gas pipe, so that the air pressure in the kettle chamber will no longer increase, thereby avoiding safety problems caused by excessive air pressure in the kettle chamber.

[0098] Preferably, the abnormal factors include an abnormality in the reactor heater causing the reactor chamber temperature to be too high.

[0099] It should be understood that within the scope of the present invention, the above-mentioned technical features of the present invention and the technical features specifically described below (such as embodiments) can be combined with each other to form new or preferred technical solutions. BRIEF DESCRIPTION OF THE DRAWINGS

[0100] It should be understood that the drawings are only used for illustrative purposes and should not be construed as limitations on this patent; in order to better illustrate this embodiment, some parts of the drawings may be omitted, enlarged or reduced, and do not represent the size of the actual product; for those skilled in the art, it is understandable that some well-known structures and their descriptions in the drawings may be omitted; the same or similar numbers correspond to the same or similar parts; the terms describing the positional relationship in the drawings are only used for illustrative purposes and should not be construed as limitations on this patent.

[0101] Figure 1 The figure is a schematic diagram of the structure of a reaction kettle in a preferred example of the utility model.

[0102] Wherein, each number in the accompanying drawings represents:

[0103] 1 is the kettle chamber, 2 is the first high-pressure gas source, 3 is the capillary, 4 is the sliding plug, 5 is the return spring, 6 is the horizontal channel, 7 is the first through hole, 8 is the second through hole, 9 is the third through hole, 10 is the first gas pipe, 11 is the second gas pipe, 12 is the third gas pipe, 13 is the valve, 14 is the material taking pipe, 15 is the sampling bottle, 16 is the fifth gas pipe and 17 is the third high-pressure gas source. DETAILED DESCRIPTION

[0104] After extensive and in-depth research, the inventors have developed a reaction kettle, which includes a kettle chamber, a pressure controller and a first high-pressure gas source. The reaction kettle can be simply and effectively used for gas-liquid phase reactions.

[0105] the term

[0106] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.

[0107] As used herein, the terms "include", "comprises", and "comprising" are used interchangeably, and include not only open definitions, but also semi-closed and closed definitions. In other words, the terms include "consisting of", "consisting essentially of".

[0108] As used herein, the terms "upper", "lower" and "bottom" etc. indicate orientations or positional relationships based on the orientations or positional relationships shown in the accompanying drawings, and are only for the convenience of describing the invention and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and therefore cannot be understood as a limitation on the invention of the utility model.

[0109] As used herein, the terms "first", "second", "third", "fourth", and "fifth" are used for descriptive purposes only and are not to be understood as indicating or implying relative importance or implicitly indicating the number of the indicated technical features. Thus, the term "first", "second", "third", "fourth", and "fifth" may explicitly or implicitly include one or more of the features.

[0110] As used herein, the terms “connected” and “connected” should be understood in a broad sense, and may refer to fixed connection or connection, detachable connection or connection, or integral connection or connection.

[0111] For the sake of convenience, the following Figure 1 To further describe the present invention, it should be understood that the accompanying drawings do not limit the scope of the present invention.

[0112] The utility model provides a reaction kettle, which comprises a kettle chamber 1, a pressure controller and a first high-pressure gas source 2;

[0113] The pressure controller comprises a capillary tube 3, one end of which is an open end, and the other end of which is a closed end. The open end of the capillary tube is communicated with the kettle cavity. A sliding plug 4 is provided in the cavity of the capillary tube. The sliding plug is sealed with the inner wall of the cavity of the capillary tube. One end of the sliding plug is connected to the inner wall of the closed end of the capillary tube through a reset spring 5. A horizontal channel 6 is provided inside the sliding plug. A first through hole 7, a second through hole 8 and a third through hole 9 are provided on the wall of the capillary tube. The first through hole and the second through hole are located above the third through hole, and the first through hole and the second through hole are located on the same horizontal plane.

[0114] The first through hole is connected to the kettle chamber through a first gas pipe 10, the second through hole is connected to the first high-pressure gas source through a second gas pipe 11, the third through hole is connected to a third gas pipe 12, and a valve 13 is provided on the second gas pipe;

[0115] When the kettle chamber is connected to the outside atmosphere, the sliding plug blocks the first through hole and the second through hole, the horizontal channel inside the sliding plug is located below the first through hole and the second through hole, and the vertical distance between the horizontal channel inside the sliding plug and the first through hole is smaller than the vertical distance between the bottom outer wall of the sliding plug and the third through hole.

[0116] The reaction kettle of the utility model can be used for gas-liquid phase reaction.

[0117] Those skilled in the art should understand that when the reactor described in the utility model is applied to a specific gas-liquid phase reaction that requires a high-pressure gas raw material, the gas pressure in the reactor cavity when the horizontal channel inside the sliding plug is connected to the first through hole and the second through hole can be achieved by adjusting factors such as the return spring (such as the elastic coefficient and stiffness) and the weight of the sliding plug to achieve the gas pressure required for the high-pressure gas raw material to react. When the gas pressure in the reactor cavity exceeds a specific value, the lumen of the capillary under the bottom of the sliding plug is connected to the third through hole. These are all conventional technical operating means in the field.

[0118] The reactor of the utility model can be simply and effectively used to realize the continuous filling of the reactor with high-pressure gas raw materials so that the gas raw materials are kept at the required high pressure for gas-liquid phase reaction and avoid the safety problems caused by excessive pressure in the reactor cavity. A typical working principle is as follows:

[0119] Specifically, the following commonly used gas-liquid phase reaction of reducing an iopamidol transester to an iopamidol reduced product is used as an example for illustration, and the reaction comprises:

[0120]

[0121] Using 9-11 atmospheres of H2 to reduce the iopamidol ester exchange product in the water solvent to an iopamidol reduction product, thereby obtaining the iopamidol reduction product;

[0122] For the gas-liquid phase reaction of reducing the iopamidol ester exchange product to the iopamidol reduction product, by adjusting factors such as the return spring (such as the elastic coefficient and stiffness) and the weight of the sliding plug, the H2 gas pressure in the kettle cavity when the horizontal channel inside the sliding plug is connected to the first through hole and the second through hole is 10 atmospheres, and when the H2 gas pressure in the kettle cavity is 12 atmospheres, the lumen of the capillary below the bottom of the sliding plug is connected to the third through hole;

[0123] The first high-pressure gas source contains H2 raw materials at 10 atmospheres, the valve on the second gas pipe is closed, and the H2 raw materials at 11 atmospheres are first filled into the kettle cavity through other high-pressure H2 sources (such as the second high-pressure gas source containing H2 raw materials at 11 atmospheres), and then the H2 filling is stopped. At this time, the horizontal channel inside the sliding plug is located above the first through hole and the second through hole, and the valve on the second gas pipe is opened. As the H2 raw materials in the reactor are continuously reacted and consumed, the H2 pressure in the kettle cavity is continuously reduced, and the sliding plug slides downward along the inner wall of the tube cavity of the capillary. When the H2 pressure in the kettle cavity drops to 10 atmospheres, the horizontal channel inside the sliding plug is closed. The passage is connected with the first through hole and the second through hole. At this time, the H2 raw material of the first high-pressure gas source is filled with the H2 raw material of 10 atmospheres into the still chamber through the second gas pipe, the horizontal channel inside the sliding plug and the second gas pipe, thereby ensuring that the H2 raw material in the still chamber is maintained at 10 atmospheres, so that H2 reacts with the iopamidol ester exchange product in the water solvent to generate the iopamidol reductant; of course, in this specific application process, the H2 raw material gas pressure of the first high-pressure gas source can also be made greater than 10 atmospheres (such as 11 atmospheres), thereby further ensuring that the H2 raw material gas pressure in the still chamber is not less than 10 atmospheres, thereby ensuring the reaction;

[0124] During the reaction process, if an abnormal factor occurs (such as an abnormality in the reactor heater causing the reactor chamber temperature to be too high, etc.), causing the pressure in the reactor chamber to continue to rise, the sliding plug slides upward along the inner wall of the tube cavity of the capillary tube. When the pressure in the reactor chamber rises to 12 atmospheres, the tube cavity of the capillary tube below the bottom of the sliding plug is connected to the third through hole, and the high-pressure gas in the reactor chamber is discharged in time through the third gas pipe, so that the pressure in the reactor chamber no longer increases, thereby avoiding safety problems caused by excessive pressure in the reactor chamber.

[0125] Therefore, the reactor of the utility model can be simply and effectively used to realize continuous filling of the reactor with high-pressure gas raw materials so that the gas raw materials are kept at the required high pressure for gas-liquid phase reaction and to avoid safety problems caused by excessive pressure in the reactor cavity.

[0126] The reactor of the utility model may also include a second high-pressure gas source. The second high-pressure gas source can be used to charge the reactor cavity with high-pressure gas raw materials before the gas-liquid phase reaction, so that the gas pressure of the gas raw materials in the reactor cavity is slightly higher than the gas pressure for the reaction.

[0127] In a preferred example of the utility model, the reactor further comprises a sampler, the sampler comprises a material taking tube and a sampling bottle, one end of the material taking tube is in communication with the reactor cavity, the other end of the material taking tube is a closed end, a valve is provided on the material taking tube, and the sampling bottle is connected to the material taking tube. The reaction liquid of the reactor can be sampled by the sampler to observe and detect the progress of the reaction, etc.

[0128] Preferably, the material taking pipe is connected to the third high-pressure gas source through a fifth gas pipe, and a valve is provided on the fifth gas pipe. In the chemical reaction process, it is often necessary to sample and observe the reaction liquid in the reactor to detect the progress of the reaction. For many gas-liquid phase reactions, solids will be produced as the reaction proceeds. In the sampling process, the solids are likely to cause the sampling pipe to be blocked, thereby causing an adverse effect on the sampling. The third high-pressure gas source performs high-pressure dredging on the material taking pipe through the fifth gas pipe, which can avoid the sampling difficulty caused by the clogging of the sampling pipe and make the sampling proceed smoothly.

[0129] In a preferred example of the present invention, the capillary tube is a transparent capillary tube, through which the sliding of the sliding plug on the inner wall of the lumen of the capillary tube and the position of the channel opening of the horizontal channel inside the sliding plug can be easily observed.

[0130] Preferably, the side wall of the capillary tube is provided with scale lines, and the gas pressure in the kettle chamber can be quantitatively indicated by the position of the bottom outer wall of the sliding plug corresponding to the scale lines.

[0131] The shapes of the first through hole, the second through hole and the third through hole described in the present invention are not particularly limited, and are preferably circular holes.

[0132] The shape of the horizontal channel inside the sliding plug of the utility model is not particularly limited, and is preferably a cylindrical channel.

[0133] The shape of the sliding plug of the present invention is not particularly limited, and is preferably a cylindrical sliding plug.

[0134] The main excellent technical effects of the utility model include:

[0135] 1. The utility model develops a reactor, which can be simply and effectively used to continuously fill the reactor with high-pressure gas raw materials so that the gas raw materials are kept at the required high pressure for gas-liquid phase reaction and avoid safety problems caused by excessive gas pressure in the reactor cavity.

[0136] 2. The reactor described in the utility model has a simple structure and is easy to industrialize.

[0137] The present invention is further described below in conjunction with specific embodiments. It should be understood that these embodiments are only used to illustrate the present invention and are not used to limit the scope of the present invention.

[0138] Example 1

[0139] This embodiment 1 provides a reaction kettle, which comprises a kettle chamber 1, a pressure controller and a first high-pressure gas source 2;

[0140] The pressure controller comprises a capillary tube 3, one end of which is an open end, and the other end of which is a closed end. The open end of the capillary tube is communicated with the kettle cavity. A sliding plug 4 is provided in the cavity of the capillary tube. The sliding plug is sealed with the inner wall of the cavity of the capillary tube. One end of the sliding plug is connected to the inner wall of the closed end of the capillary tube through a reset spring 5. A horizontal channel 6 is provided inside the sliding plug. A first through hole 7, a second through hole 8 and a third through hole 9 are provided on the wall of the capillary tube. The first through hole and the second through hole are located above the third through hole, and the first through hole and the second through hole are located on the same horizontal plane.

[0141] The first through hole is connected to the kettle chamber through a first gas pipe 10, the second through hole is connected to the first high-pressure gas source through a second gas pipe 11, the third through hole is connected to a third gas pipe 12, and a valve 13 is provided on the second gas pipe;

[0142] When the kettle chamber is connected to the outside atmosphere, the sliding plug blocks the first through hole and the second through hole, the horizontal channel inside the sliding plug is located below the first through hole and the second through hole, and the vertical distance between the horizontal channel inside the sliding plug and the first through hole is smaller than the vertical distance between the bottom outer wall of the sliding plug and the third through hole.

[0143] The reactor described in the utility model can be used for gas-liquid phase reaction, and the factors such as the elastic coefficient and stiffness of the return spring and the weight of the sliding plug can be adjusted to achieve the gas pressure in the reactor cavity when the horizontal channel inside the sliding plug is connected with the first through hole and the second through hole to be the gas pressure of the required high-pressure gas raw material for reaction, and the first high-pressure gas source containing the required high-pressure gas raw material is filled into the reactor cavity through the second gas pipe, the horizontal channel inside the sliding plug and the second gas pipe, so that the reaction continues; when the gas pressure in the reactor cavity exceeds a specific value, the lumen of the capillary tube under the bottom of the sliding plug is connected with the third through hole, and the high-pressure gas in the reactor cavity will be discharged in time through the third gas pipe, so that the gas pressure in the reactor cavity no longer increases, thereby avoiding safety problems caused by excessive gas pressure in the reactor cavity.

[0144] The above description is only the preferred embodiment of the present application and is not intended to limit the present application. For those skilled in the art, the present application may have various modifications and variations. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present application shall be included in the protection scope of the present application.

Claims

1. A reaction kettle, characterized in that: The reaction kettle comprises a kettle chamber (1), a pressure controller and a first high-pressure gas source (2); The pressure controller comprises a capillary tube (3), one end of the capillary tube is an open end, and the other end of the capillary tube is a closed end. The open end of the capillary tube is in communication with the kettle chamber. A sliding plug (4) is provided in the tube chamber of the capillary tube. The sliding plug is sealedly connected to the inner wall of the tube chamber of the capillary tube. One end of the sliding plug is connected to the inner wall of the closed end of the capillary tube via a return spring (5). A horizontal channel (6) is provided inside the sliding plug. A first through hole (7), a second through hole (8) and a third through hole (9) are provided on the tube wall of the capillary tube. The first through hole and the second through hole are located above the third through hole. The first through hole and the second through hole are located on the same horizontal plane. The first through hole is connected to the kettle chamber via a first gas pipe (10), the second through hole is connected to the first high-pressure gas source via a second gas pipe (11), the third through hole is connected to a third gas pipe (12), and a valve (13) is provided on the second gas pipe; When the kettle chamber is connected to the outside atmosphere, the sliding plug blocks the first through hole and the second through hole, the horizontal channel inside the sliding plug is located below the first through hole and the second through hole, and the vertical distance between the horizontal channel inside the sliding plug and the first through hole is smaller than the vertical distance between the bottom outer wall of the sliding plug and the third through hole.

2. The reactor according to claim 1, characterized in that: When the kettle cavity is communicated with the outside atmosphere, the horizontal channel inside the sliding plug is located above the third through hole.

3. The reactor according to claim 1, characterized in that: The reactor further comprises a sampler, which comprises a material taking tube (14) and a sampling bottle (15). One end of the material taking tube is in communication with the reactor cavity, and the other end of the material taking tube is a closed end. A valve (13) is provided on the material taking tube, and the sampling bottle is connected to the material taking tube.

4. The reactor according to claim 3, characterized in that: The material taking pipe is connected to a third high-pressure gas source (17) via a fifth gas pipe (16), and a valve (13) is provided on the fifth gas pipe.

5. The reactor according to claim 1, characterized in that: The capillary comprises a cylindrical tube.

6. The reactor according to claim 1, characterized in that: The capillary is a transparent capillary.

7. The reactor according to claim 1, characterized in that: The sliding plug is a cylindrical sliding plug.

8. The reactor according to claim 1, characterized in that: The first through hole and the second through hole are both circular holes.

9. The reactor according to claim 1, characterized in that: The first through hole and the second through hole are the same hole.

10. The reactor according to claim 1, characterized in that: The channel opening of the horizontal channel inside the sliding plug is the same as the holes of the first through hole and the second through hole.

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