Liquid-solid separation reaction kettle system and liquid-solid separation method

Abstract

The invention relates to the technical field of liquid-solid separation reaction, and discloses a liquid-solid separation reaction kettle system and a liquid-solid separation method. The liquid-solid separation reaction kettle system comprises a high-pressure reaction kettle, a solution metering liquid inlet system, a catalyst metering liquid inlet system, a low-pressure nitrogen feeding system, a high-pressure nitrogen feeding system, a temperature control circulating system, an emptying system and a vacuumizing system, and a balance pipe is arranged in a kettle cover of the high-pressure reaction kettle; a balance hole communicated with the gas environment in the high-pressure reaction kettle is formed in the upper part of the balance pipe; a liquid level meter for detecting the liquid level in the kettle is mounted in the balance pipe; the bottom end of the balance pipe is flush with the lower bottom of the straight barrel section of the high-pressure reaction kettle, or the bottom end of the balance pipe is lower than the lower bottom of the straight barrel section of the high-pressure reaction kettle. The liquid level in the balance pipe is the same as the liquid level in the high-pressure reaction kettle, and the balance pipe can effectively reduce the influence of stirring on the liquid level, so that the liquid level in the kettle can be detected by measuring the liquid level of the balance pipe, and the measurement accuracy of the liquid level in the kettle is improved.

Description

Technical Field

[0001] The present invention relates to the technical field of liquid-solid separation reaction, and more specifically to a liquid-solid separation reactor system. In addition, the present invention also provides a liquid-solid separation method for the liquid-solid separation reactor system. Background Art

[0002] In the production process of traditional liquid-solid separation reactors, the liquid level inside the high-pressure reactor is mostly converted through the feed amount and recovery amount of the material. The conventional liquid level measurement method is to install a differential pressure level gauge on the side or end face of the high-pressure reactor to measure the liquid level.

[0003] However, in the process of measuring the liquid level inside the high-pressure reactor, since the liquid level in the high-pressure reactor is always changing and as the liquid level gradually decreases, the proportion of solid powder in the reactor gradually increases, causing the density of the medium in the reactor to change, resulting in inaccurate measurement of the differential pressure level gauge, which seriously affects the accurate judgment of the actual material in the reactor, and further leads to energy waste and incomplete product separation.

[0004] In summary, how to improve the measurement accuracy of the liquid level in the high-pressure reactor is a problem that needs to be solved urgently by those skilled in the art. Summary of the invention

[0005] In view of this, the object of the present invention is to provide a liquid-solid separation reactor system, in which the liquid level in the balance tube is the same as the liquid level in the reactor of the high-pressure reactor, and the balance tube can effectively reduce the influence of stirring on the liquid level. The liquid level in the reactor can be detected by measuring the liquid level in the balance tube, thereby improving the measurement accuracy of the liquid level in the reactor.

[0006] In addition, the present invention also provides a liquid-solid separation method for the above-mentioned liquid-solid separation reactor system.

[0007] In order to achieve the above object, the present invention provides the following technical solutions:

[0008] A liquid-solid separation reactor system, comprising a high-pressure reactor, a solution metering liquid inlet system, a catalyst metering liquid inlet system, a low-pressure nitrogen feeding system, a high-pressure nitrogen feeding system, a temperature control circulation system, a venting system and a vacuum system, wherein a balance pipe is provided inside a reactor cover of the high-pressure reactor, a balance hole is provided on the upper part of the balance pipe and is connected to the gas environment in the high-pressure reactor, and a liquid level gauge for detecting the liquid level in the reactor is installed in the balance pipe;

[0009] The bottom end of the balance pipe is flush with the lower bottom of the straight section of the high-pressure reactor, or the bottom end of the balance pipe is lower than the lower bottom of the straight section of the high-pressure reactor.

[0010] Preferably, the low-pressure nitrogen feed system and the high-pressure nitrogen feed system are both connected to the high-pressure reactor through a nitrogen purge system, and the nitrogen purge system comprises a nitrogen purge pipe and an aeration pipe arranged at the bottom of the high-pressure reactor, one end of the nitrogen purge pipe is connected to the low-pressure nitrogen feed system and the high-pressure nitrogen feed system, and the other end of the nitrogen purge pipe is connected to the aeration pipe.

[0011] Preferably, the aeration pipe comprises an aeration coil, the axis of the aeration coil is colinear with the axis of the stirring paddle inside the high-pressure reactor, and the aeration coil is evenly provided with a plurality of aeration holes along the circumferential direction.

[0012] Preferably, it also includes a cleaning liquid inlet system for cleaning the balancing pipe, the cleaning liquid inlet system includes a cleaning liquid inlet pipe, the cleaning liquid inlet pipe is connected to the balancing pipe so as to introduce the cleaning liquid into the balancing pipe, and the cleaning liquid inlet pipe is provided with a cleaning feed valve for controlling the on-off of the pipeline.

[0013] Preferably, the cleaning feed valve comprises a cleaning feed ball valve, and the cleaning feed ball valve is used to adjust the flow rate of the cleaning liquid inlet pipeline.

[0014] Preferably, the outer peripheral surface of the balance pipe is provided with an external thread, and the balance pipe thread is installed in the balance pipe installation hole of the kettle cover.

[0015] Preferably, the liquid level meter comprises a radar liquid level meter, and the radar liquid level meter is arranged above the kettle cover.

[0016] A liquid-solid separation method, used in any of the above-mentioned liquid-solid separation reactor systems, comprising:

[0017] The high-pressure reactor is replaced with nitrogen, and the replaced high-pressure reactor is emptied and vacuumized;

[0018] Adding the raw material solution and the catalyst into the autoclave, and adjusting the temperature inside the autoclave to a preset reaction temperature;

[0019] When the pressure inside the autoclave of the high-pressure reactor is controlled to decrease to a preset slightly positive pressure value, the temperature inside the autoclave of the high-pressure reactor is adjusted to a preset separation control temperature, and high-pressure nitrogen is introduced into the autoclave to perform liquid-solid separation control;

[0020] When the fluctuation value of the liquid level in the reactor measured by the liquid level meter is less than the preset fluctuation value, the solid powder in the high-pressure reactor is discharged;

[0021] After the solid powder is discharged, the balance pipe is cleaned and the waste liquid after cleaning is discharged.

[0022] Preferably, the cleaning of the balance pipe and discharging of the cleaned waste liquid comprises:

[0023] Control the shutdown of the low-pressure nitrogen feeding system and the vacuum system;

[0024] Adjust the temperature control circulation system to adjust the temperature in the kettle to a preset cleaning temperature;

[0025] Controlling the cleaning liquid inlet system to open, and passing the cleaning liquid into the balance pipe;

[0026] The bottom valve at the bottom of the high-pressure reactor is controlled to open to discharge the cleaned waste liquid.

[0027] Preferably, the step of replacing the high-pressure reactor with nitrogen and emptying and evacuating the high-pressure reactor after the replacement comprises:

[0028] Controlling the low-pressure nitrogen feeding system to open, and introducing low-pressure nitrogen into the high-pressure reactor;

[0029] When the pressure in the kettle rises to a preset emptying value, the low-pressure nitrogen feeding system is controlled to be closed and the venting system is controlled to be opened;

[0030] When the pressure in the kettle drops to the preset slightly positive pressure value, the venting system is controlled to be closed and the vacuum system is controlled to be opened;

[0031] When the pressure in the kettle drops to a preset negative pressure value, the vacuum system is controlled to be closed.

[0032] In the liquid-solid separation reactor system provided by the present invention, the bottom end of the balance pipe is flush with or lower than the lower end of the straight cylinder section of the high-pressure reactor, and the balance pipe can be connected with the gas environment in the high-pressure reactor through the balance hole. The balance pipe and the high-pressure reactor constitute a communicating vessel, so that the liquid level in the balance pipe is always the same as the liquid level in the kettle of the high-pressure reactor. At the same time, the balance pipe can effectively reduce the influence of stirring on the liquid level, thereby improving the accuracy of the liquid level meter in measuring the liquid level in the kettle, providing a reliable basis for test personnel to accurately judge the actual material in the kettle, and avoiding the problems of energy waste and incomplete product separation caused by inaccurate measurement of the liquid level in the kettle.

[0033] In addition, the present invention also provides a liquid-solid separation method for the above-mentioned liquid-solid separation reactor system, which can separate products thoroughly and save energy. BRIEF DESCRIPTION OF THE DRAWINGS

[0034] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required for use in the embodiments or the description of the prior art will be briefly introduced below. Obviously, the drawings described below are only embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on the provided drawings without paying creative work.

[0035] Figure 1 This is a schematic structural diagram of a specific embodiment of the liquid-solid separation reactor system provided by the present invention.

[0036] Figure 1 middle:

[0037] 10-high pressure reactor; 101-balance pipe; 1011-liquid level gauge; 1012-balance hole; 102-temperature sensor; 103-pressure transmitter; 104-pressure gauge; 105-bottom valve; 20-solution metering inlet system; 30-catalyst metering inlet system; 40-low pressure nitrogen feeding system; 50-high pressure nitrogen feeding system; 60-nitrogen purge system; 601-nitrogen purge pipe; 602-aeration pipe; 70-venting system; 80-vacuuming system; 90-cleaning inlet system; 901-cleaning feed valve; 100-temperature control circulation system. DETAILED DESCRIPTION

[0038] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0039] The core of the present invention is to provide a liquid-solid separation reactor system, in which the liquid level in the balance tube is the same as the liquid level in the reactor of the high-pressure reactor, and the balance tube can effectively reduce the influence of stirring on the liquid level. The liquid level in the reactor can be detected by measuring the liquid level in the balance tube, thereby improving the measurement accuracy of the liquid level in the reactor.

[0040] In addition, the present invention also provides a liquid-solid separation method for the above-mentioned liquid-solid separation reactor system.

[0041] The liquid-solid separation reactor system provided by the present invention comprises a high-pressure reactor 10, a solution metering liquid inlet system 20, a catalyst metering liquid inlet system 30, a low-pressure nitrogen feeding system 40, a high-pressure nitrogen feeding system 50, a temperature control circulation system 100, a venting system 70 and a vacuum pumping system 80. A balance pipe 101 is provided inside the reactor cover of the high-pressure reactor 10. A balance hole 1012 communicating with the gas environment in the high-pressure reactor 10 is provided on the upper part of the balance pipe 101. A liquid level gauge 1011 for detecting the liquid level in the reactor is installed in the balance pipe 101.

[0042] The bottom end of the balance pipe 101 is flush with the lower bottom of the straight section of the autoclave 10 , or the bottom end of the balance pipe 101 is lower than the lower bottom of the straight section of the autoclave 10 .

[0043] Please refer to Figure 1The high-pressure reactor 10 is connected and communicated with the solution metering liquid inlet system 20, the catalyst metering liquid inlet system 30 and the high-pressure nitrogen feeding system 50 so as to introduce the raw material solution, the catalyst and the high-pressure nitrogen into the high-pressure reactor 10; the solution metering liquid inlet system 20, the catalyst metering liquid inlet system 30 and the high-pressure nitrogen feeding system 50 are all provided with a one-way valve for controlling the one-way flow of the pipeline and a flow regulating valve for controlling the flow rate of the pipeline.

[0044] The high-pressure reactor 10 is connected to a low-pressure nitrogen feeding system 40, a venting system 70 and a vacuuming system 80, wherein the low-pressure nitrogen feeding system 40 can cooperate with the venting system 70 to discharge the gas in the high-pressure reactor 10 and replace the high-pressure reactor 10 with nitrogen, and the vacuuming system 80 is used to draw a negative pressure on the high-pressure reactor 10 after it is emptied to meet the actual reaction needs;

[0045] The low-pressure nitrogen feed system 40 is provided with a one-way valve for controlling one-way flow in the pipeline and a flow regulating valve for controlling the flow rate in the pipeline, while the venting system 70 and the vacuum system 80 are mainly provided with a flow control valve for controlling the flow rate in the pipeline or a stop valve for controlling the on-off of the pipeline.

[0046] The jacket of the high-pressure reactor 10 is connected to the temperature control circulation system 100. By adjusting the temperature and flow rate of the temperature control water entering and flowing out of the jacket, the temperature inside the high-pressure reactor 10 can be adjusted to meet the temperature control requirements of different stages of the liquid-solid separation reaction; the water inlet circuit and the return circuit of the temperature control circulation system 100 are both provided with flow control valves for controlling the pipeline flow.

[0047] The high-pressure reactor 10 is provided with a level gauge 1011 for detecting the liquid level in the reactor, a temperature sensor 102 for detecting the temperature in the reactor, and a pressure transmitter 103 and a pressure gauge 104 for detecting the pressure in the reactor. The specific types, models and installation methods of the temperature sensor 102, the pressure transmitter 103 and the pressure gauge 104 can be determined according to the actual reaction needs with reference to the existing technology.

[0048] In order to increase the rate of the solid-liquid separation reaction, a stirring paddle is provided inside the high-pressure reactor 10 to stir the raw material solution, catalyst and solid powder. The stirring causes the liquid level in the high-pressure reactor 10 to fluctuate, affecting the accuracy of liquid level detection.

[0049] In order to reduce the influence of stirring on liquid level detection, a balance pipe 101 is provided on the lid of the autoclave 10, and the balance pipe 101 and the autoclave 10 form a communicating vessel to ensure that the liquid level in the balance pipe 101 is consistent with the liquid level in the autoclave 10, so that the liquid level meter 1011 measures the liquid level in the autoclave by measuring the liquid level in the balance pipe 101;

[0050] It is understandable that the liquid level gauge 1011 is installed in the balance pipe 101 , and the outer diameter of the liquid level gauge 1011 is the same as the inner diameter of the balance pipe to prevent the gas in the high-pressure reactor 10 from leaking outward from the gap between the liquid level gauge 1011 and the balance pipe 101 .

[0051] The balancing tube 101 can be installed in the balancing tube mounting hole of the kettle cover by interference fit, or can be connected to the kettle cover by threaded connection, flange connection, etc. Usually, the outer peripheral surface of the balancing tube 101 is provided with an external thread, and the balancing tube 101 is threadedly installed in the balancing tube mounting hole of the kettle cover. The connection is stable and reliable, the connection is highly sealed, and the connection method is simple and easy to process and disassemble.

[0052] In order to enable the balance pipe 101 to form a communicating vessel with the autoclave 10, on the one hand, the bottom end of the balance pipe 101 should be lower than the lowest liquid level in the autoclave 10, otherwise the balance pipe 101 may be completely suspended above the liquid level of the autoclave 10, and the balance pipe 101 loses its inhibitory effect on stirring fluctuations. Therefore, the bottom end of the balance pipe 101 needs to be flush with the lower bottom of the straight section of the autoclave 10, or lower than the lower bottom of the straight section of the autoclave 10;

[0053] In order to prevent the bottom end of the balance pipe 101 from contacting the curved bottom of the autoclave 10 and to ensure the circulation and balance of the materials in the autoclave 10 , the bottom end of the balance pipe 101 is usually directly arranged to be flush with the lower bottom of the straight cylinder section of the autoclave 10 .

[0054] On the other hand, the balance pipe 101 needs to be connected to the gas environment in the high-pressure reactor 10 to avoid a liquid level difference between the two due to the pressure gradient of the gas environment. Therefore, a balance hole 1012 for connecting to the gas environment in the high-pressure reactor 10 is provided on the upper part of the balance pipe 101.

[0055] The number, shape and size of the balancing holes 1012 are not limited as long as they can connect the gas environment inside and outside the balancing tube 101 ; the balancing holes 1012 are preferably configured as circular holes to facilitate the processing of the balancing holes 1012 on the balancing tube 101 .

[0056] The specific type and model of the liquid level meter 1011 can be determined according to the actual reaction needs, such as the requirements for liquid level measurement accuracy. The liquid level meter 1011 is usually set as a radar level meter, which is installed above the kettle cover and connected to the refined hexane or cleaning solution. It measures the liquid level in the balance tube 101 in a non-contact manner and has a long service life.

[0057] In this embodiment, the bottom end of the balancing tube 101 is flush with or lower than the lower end of the straight section of the high-pressure reactor 10, and the balancing tube 101 can be connected to the gas environment in the high-pressure reactor 10 through the balancing hole 1012. The balancing tube 101 and the high-pressure reactor 10 constitute a communicating vessel, so that the liquid level in the balancing tube 101 is always the same as the liquid level in the kettle of the high-pressure reactor 10. At the same time, the balancing tube 101 can effectively reduce the influence of stirring on the liquid level, thereby improving the accuracy of the liquid level meter 1011 in measuring the liquid level in the kettle, providing a reliable basis for the test personnel to accurately judge the actual material in the kettle, and avoiding the problems of energy waste and incomplete product separation caused by inaccurate measurement of the liquid level in the kettle.

[0058] Preferably, a seal such as a fluororubber sealing ring is provided between the inner circumference of the balance pipe 101 and the outer circumference of the liquid level gauge 1011. The seal is used to seal the gap between the balance pipe 101 and the liquid level gauge 1011, further improving the air tightness of the installation location of the liquid level gauge 1011.

[0059] On the basis of the above embodiment, the low-pressure nitrogen feeding system 40 and the high-pressure nitrogen feeding system 50 are both connected to the high-pressure reactor 10 through the nitrogen purge system 60. The nitrogen purge system 60 includes a nitrogen purge pipe 601 and an aeration pipe 602 arranged at the bottom of the high-pressure reactor 10. One end of the nitrogen purge pipe 601 is connected to the low-pressure nitrogen feeding system 40 and the high-pressure nitrogen feeding system 50, and the other end of the nitrogen purge pipe 601 is connected to the aeration pipe 602.

[0060] The nitrogen purge pipe 601 can be connected to the low-pressure nitrogen feed system 40 and the high-pressure nitrogen feed system respectively, or can be connected to the low-pressure nitrogen feed system 40 and the high-pressure nitrogen feed system respectively. Figure 1 As shown, it is directly connected to the feed main pipes of the two to simplify the pipeline layout; the specific connection method of the nitrogen purge pipe 601 with the low-pressure nitrogen feed system 40 and the high-pressure nitrogen feed system 50 can be determined according to the actual reaction needs with reference to the existing technology, such as quick-connect connection, threaded connection, etc.

[0061] The aeration pipe 602 is disposed at the bottom of the high-pressure reactor 10 and is used to pass low-pressure nitrogen or high-pressure nitrogen into the high-pressure reactor 10. Compared with ordinary pipelines, the aeration pipe 602 is usually provided with multiple aeration holes, which can increase the contact area between the gas and the reactants inside the high-pressure reactor 10 and improve the uniformity of the gas distribution in the high-pressure reactor 10.

[0062] Please refer to Figure 1 The aeration pipe 602 is preferably configured as an aeration coil, the axis of the aeration coil is colinear with the axis of the stirring paddle inside the high-pressure reactor 10, and the aeration coil is evenly provided with a plurality of aeration holes along the circumferential direction to improve the air intake uniformity of the high-pressure reactor 10.

[0063] In this embodiment, the nitrogen purge system 60 can realize the dispersed air intake of the high-pressure reactor 10. Compared with the centralized air intake design of the ordinary pipeline, it is beneficial to improve the air intake uniformity of the high-pressure reactor 10 and facilitate the separation of the solid powder in the high-pressure reactor 10 with stirring.

[0064] On the basis of the above embodiment, it also includes a cleaning liquid inlet system 90 for cleaning the balance pipe 101. The cleaning liquid inlet system 90 includes a cleaning liquid inlet pipeline. The cleaning liquid inlet pipeline is connected to the balance pipe 101 so as to introduce the cleaning liquid into the balance pipe 101. The cleaning liquid inlet pipeline is provided with a cleaning feed valve 901 for controlling the on-off of the pipeline.

[0065] Considering that most of the pipeline of the balance pipe 101 in the high-pressure reactor 10 is immersed in the raw material solution, in order to prevent the residual liquid on the inner wall of the balance pipe 101 from affecting the subsequent liquid level measurement, the balance pipe 101 needs to be cleaned after the reaction is completed;

[0066] Since the liquid level gauge 1011 is a non-contact liquid level gauge, the connection point between the cleaning liquid inlet pipeline and the balance pipe 101 is lower than the liquid level gauge 1011 to prevent the cleaning liquid from contacting the liquid level gauge 1011 and affecting the normal function of the liquid level gauge 1011.

[0067] The cleaning liquid inlet pipeline is provided with a cleaning feed valve 901. After the discharge of the solid-liquid separation reaction is completed, the cleaning feed valve 901 is controlled to open, and the cleaning liquid enters the balance pipe 101 through the cleaning liquid inlet pipeline to clean the inner wall surface of the balance pipe 101; and after the cleaning is completed, the cleaning feed valve 901 is controlled to close.

[0068] Preferably, the cleaning feed valve 901 may include a cleaning feed ball valve. Compared with an ordinary stop valve, the cleaning feed ball valve can adjust the flow of the cleaning liquid inlet pipeline, so as to adjust the flow of the cleaning liquid inlet pipeline according to actual needs, thereby reducing the cleaning cost.

[0069] In addition to the above-mentioned liquid-solid separation reactor system, the present invention also provides a liquid-solid separation method for the liquid-solid separation reactor system disclosed in the above-mentioned embodiment, comprising:

[0070] Step S1, replacing the high-pressure reactor 10 with nitrogen, and emptying and evacuating the high-pressure reactor 1 after the replacement;

[0071] Step S2, adding the raw material solution and the catalyst into the autoclave 10, and adjusting the temperature inside the autoclave 10 to a preset reaction temperature;

[0072] Step S3, when the pressure in the autoclave of the high-pressure reactor 10 is controlled to be reduced to a preset slightly positive pressure value, the temperature in the autoclave of the high-pressure reactor 10 is adjusted to a preset liquid-solid separation control temperature, and high-pressure nitrogen is introduced into the autoclave 10 to perform liquid-solid separation control;

[0073] Step S4, when the fluctuation value of the liquid level in the autoclave measured by the liquid level meter 1011 is less than the preset fluctuation value, the solid powder in the high-pressure reactor 10 is discharged;

[0074] Step S5, after the solid powder is discharged, the balance pipe 101 is cleaned and the waste liquid after cleaning is discharged.

[0075] It is necessary to explain step S1 that before adding the raw material solution and the catalyst, the original gas in the high-pressure reactor 10 needs to be replaced by low-pressure nitrogen and the pressure in the high-pressure reactor 10 needs to be adjusted to negative pressure by the vacuum system 80 to meet the feeding requirements of the high-pressure reactor 10;

[0076] In order to meet the above-mentioned feeding requirements, it is necessary to control the low-pressure nitrogen feeding system 40 to open and introduce low-pressure nitrogen into the high-pressure reactor 10; when the pressure transmitter 103 and / or the pressure gauge 104 detects that the pressure in the reactor rises to a preset emptying value, usually the pressure in the reactor When the pressure in the reactor drops to a preset micro-positive pressure value, the pressure in the reactor is usually When the pressure in the kettle drops to a preset negative pressure value, the pressure in the kettle is usually When the pressure is -100 KPa, it can be considered that the high-pressure reactor 10 is close to a vacuum state, and the vacuum pumping system 80 is controlled to be closed.

[0077] It can be understood that the pressure inside the autoclave 10 is related to the temperature inside the autoclave. Therefore, before nitrogen replacement, it is necessary to adjust the temperature control circulation system 100 to stabilize the temperature inside the autoclave at a specific preset nitrogen replacement temperature, usually 15°C; the above-mentioned preset emptying value, preset slightly positive pressure value, preset negative pressure value and preset nitrogen replacement temperature are not fixed values ​​and can be adjusted according to actual reaction needs.

[0078] It should be explained that step S2 controls the solution metering liquid inlet system 20 and the catalyst metering liquid inlet system 30 to be opened, and the raw material solution and the catalyst are added into the autoclave 10. The specific types, dosages and proportions of the raw material solution and the catalyst to be added need to be determined according to the actual reaction requirements.

[0079] When the dosage of the raw material solution and the catalyst reaches the preset dosage, the solution metering liquid inlet system 20 and the catalyst metering liquid inlet system 30 are controlled to be closed.

[0080] It should be noted that step S3 is that after the reaction of the raw material solvent is basically completed, the pressure in the autoclave 10 is controlled to gradually decrease, usually by reducing the pressure in the autoclave 10 through the venting system 70. When the pressure in the autoclave is reduced to a preset slight positive pressure value, the pressure in the autoclave is usually When the pressure is 0.02MPa, in order to avoid waste of the raw material solution, the temperature control circulation system 100 is controlled to make the temperature inside the autoclave 10 reach the preset separation control temperature, and the high-pressure nitrogen feeding system 50 and the vacuum system 80 are controlled to be opened, and high-pressure nitrogen is introduced into the autoclave 10 to perform liquid-solid separation control in the autoclave 10.

[0081] It is necessary to explain step S4 that when the fluctuation value of the liquid level in the autoclave measured by the liquid level meter 1011 is less than the preset fluctuation value, that is, the display value of the liquid level meter 1011 is in a static state or the fluctuation value is extremely small, it can be considered that the raw material solution in the autoclave 10 has been completely recovered, and only solid powder is left in the autoclave 10, which can be discharged through the bottom valve 105 at the bottom of the autoclave 10.

[0082] It is understandable that before discharging the fixed powder, it is necessary to control the high-pressure nitrogen feed system 50 to be closed and the low-pressure nitrogen feed system 40 to be opened. When the pressure in the kettle is a slightly positive pressure value, the bottom valve 105 is controlled to open to discharge the fixed powder.

[0083] It should be explained in step S5 that in order to prevent the residual liquid from affecting the subsequent use of the balancing pipe 101, the balancing pipe 101 needs to be cleaned and the waste liquid after cleaning needs to be discharged.

[0084] The cleaning and waste discharge process of the balance pipe 101 specifically includes:

[0085] First, the low-pressure nitrogen feeding system 40 and the vacuum system 80 are controlled to be closed; then the temperature control circulation system 100 is adjusted to adjust the temperature inside the autoclave 10 to a preset cleaning temperature, usually 20°C or below; then the cleaning liquid inlet system 90 is controlled to be opened to pass the cleaning liquid into the balance pipe 101 to clean the balance pipe 101; finally, the bottom valve 105 at the bottom of the autoclave 10 is controlled to be opened to discharge the waste liquid after cleaning.

[0086] In this embodiment, the raw material solution in the high-pressure reactor 10 can be completely recovered, and the high-pressure reactor 10 can be quickly controlled to stop working after the raw material solution is completely recovered, which not only achieves complete separation of products but also avoids energy waste.

[0087] The various embodiments in this specification are described in a progressive manner, and each embodiment focuses on the differences from other embodiments. The same or similar parts between the various embodiments can be referenced to each other.

[0088] The above is a detailed introduction to the liquid-solid separation reactor system and the liquid-solid separation method provided by the present invention. Specific examples are used herein to illustrate the principles and implementation methods of the present invention. The description of the above embodiments is only used to help understand the method of the present invention and its core idea. It should be pointed out that for ordinary technicians in this technical field, without departing from the principles of the present invention, the present invention can also be improved and modified in a number of ways, and these improvements and modifications also fall within the scope of protection of the claims of the present invention.

Claims

1. A liquid-solid separation reactor system, comprising a high-pressure reactor (10), a solution metering inlet system (20), a catalyst metering inlet system (30), a low-pressure nitrogen feeding system (40), a high-pressure nitrogen feeding system (50), a temperature control circulation system (100), a venting system (70) and a vacuum pumping system (80), characterized in that: A balance pipe (101) is provided inside the lid of the high-pressure reactor (10), a balance hole (1012) is provided at the upper portion of the balance pipe (101) and is communicated with the gas environment inside the high-pressure reactor (10), and a liquid level meter (1011) for detecting the liquid level in the reactor is installed inside the balance pipe (101); The bottom end of the balance pipe (101) is flush with the lower bottom of the straight section of the high-pressure reactor (10), or the bottom end of the balance pipe (101) is lower than the lower bottom of the straight section of the high-pressure reactor (10).

2. The liquid-solid separation reactor system according to claim 1, characterized in that: The low-pressure nitrogen feeding system (40) and the high-pressure nitrogen feeding system (50) are both connected to the high-pressure reactor (10) via a nitrogen purge system (60); the nitrogen purge system (60) comprises a nitrogen purge pipe (601) and an aeration pipe (602) arranged at the bottom of the high-pressure reactor (10); one end of the nitrogen purge pipe (601) is connected to the low-pressure nitrogen feeding system (40) and the high-pressure nitrogen feeding system (50); and the other end of the nitrogen purge pipe (601) is connected to the aeration pipe (602).

3. The liquid-solid separation reactor system according to claim 2, characterized in that: The aeration pipe (602) comprises an aeration coil, the axis of the aeration coil is colinear with the axis of the stirring paddle inside the high-pressure reactor (10), and the aeration coil is evenly provided with a plurality of aeration holes along the circumferential direction.

4. The liquid-solid separation reactor system according to any one of claims 1 to 3, characterized in that: The invention also comprises a cleaning liquid inlet system (90) for cleaning the balancing pipe (101), wherein the cleaning liquid inlet system (90) comprises a cleaning liquid inlet pipeline, wherein the cleaning liquid inlet pipeline is connected to the balancing pipe (101) so as to introduce cleaning liquid into the balancing pipe (101), and the cleaning liquid inlet pipeline is provided with a cleaning feed valve (901) for controlling the on-off of the pipeline.

5. The liquid-solid separation reactor system according to claim 4, characterized in that: The cleaning feed valve (901) comprises a cleaning feed ball valve, and the cleaning feed ball valve is used to adjust the flow rate of the cleaning liquid inlet pipeline.

6. The liquid-solid separation reactor system according to any one of claims 1 to 3, characterized in that: The outer peripheral surface of the balance pipe (101) is provided with an external thread, and the balance pipe (101) is threadedly installed in the balance pipe installation hole of the kettle cover.

7. The liquid-solid separation reactor system according to any one of claims 1 to 3, characterized in that: The liquid level meter (1011) comprises a radar liquid level meter, and the radar liquid level meter is arranged above the kettle cover.

8. A liquid-solid separation method, used in the liquid-solid separation reactor system according to any one of claims 1 to 7, characterized in that: include: The high-pressure reactor (10) is replaced with nitrogen, and the high-pressure reactor (10) after the replacement is emptied and evacuated; Adding a raw material solution and a catalyst into the high-pressure reactor (10), and adjusting the temperature inside the high-pressure reactor (10) to a preset reaction temperature; Controlling the pressure inside the autoclave (10) to decrease to a preset slightly positive pressure value, adjusting the temperature inside the autoclave (10) to a preset separation control temperature, and introducing high-pressure nitrogen into the autoclave (10) to perform liquid-solid separation control; When the fluctuation value of the liquid level in the autoclave measured by the liquid level meter (1011) is less than a preset fluctuation value, the solid powder in the high-pressure reaction autoclave (10) is discharged; After the solid powder is discharged, the balance pipe (101) is cleaned and the waste liquid after cleaning is discharged.

9. The liquid-solid separation method according to claim 8, characterized in that: The cleaning of the balance pipe (101) and discharge of the waste liquid after cleaning comprises: Controlling the low-pressure nitrogen feeding system (40) and the vacuum pumping system (80) to be closed; Regulating the temperature control circulation system (100) to adjust the temperature in the kettle to a preset cleaning temperature; Controlling the cleaning liquid inlet system (90) to open, and allowing the cleaning liquid to flow into the balance pipe (101); The bottom valve (105) at the bottom of the high-pressure reactor (10) is controlled to open to discharge the waste liquid after cleaning.

10. The liquid-solid separation method according to claim 8, characterized in that: The step of replacing the high-pressure reactor (10) with nitrogen and emptying and evacuating the high-pressure reactor (10) after the replacement comprises: Controlling the low-pressure nitrogen feeding system (40) to open, and introducing low-pressure nitrogen into the high-pressure reactor (10); When the pressure in the kettle rises to a preset emptying value, the low-pressure nitrogen feeding system is controlled to be closed and the venting system (70) is opened; When the pressure in the kettle drops to the preset slightly positive pressure value, the venting system (70) is controlled to be closed and the vacuum system (80) is controlled to be opened; When the pressure in the kettle drops to a preset negative pressure value, the vacuum pumping system (80) is controlled to be closed.

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