Crude adipic acid crystallization point detection system

By improving the structure of the crystallization point detection tank and optimizing the detection sequence, combined with an automatic detection system, the problems of continuity and stability in the detection of crystallization points of crude adipic acid were solved, ensuring the stability of crude adipic acid production and the high quality of refined adipic acid products.

CN223581835UActive Publication Date: 2025-11-21HENAN SHENMA NYLON CHEM CO LTD +1
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Patent Information

Application Number
CN202520324774.3
Authority / Receiving Office
CN · China
Patent Type
Utility models(China)
Current Assignee / Owner
Filing Date
2025-02-27
Publication Date
2025-11-21
Estimated Expiration
2035-02-27

AI Technical Summary

Technical Problem

Existing crude adipic acid crystallization point detection systems suffer from problems such as poor continuity, nitrite gas escape, easy material leakage, and large errors in detection data, which affect the stability of crude adipic acid production and the accuracy of refining and purification processes.

Method used

By improving the structure of the crystallization point detection tank and optimizing the automatic feeding and detection sequence, an automatic crystallization point detection sequence controller is adopted, combined with a thermometer, an electrode-type liquid level alarm controller, a cooling water system, and a low-pressure steam system, to achieve continuous and stable detection of the crystallization point of crude adipic acid solution.

Benefits of technology

It enables continuous and stable detection of crystallization points in crude adipic acid production, providing reliable data support and ensuring the stable operation of the equipment and the high quality of refined adipic acid products.

✦ Generated by Eureka AI based on patent content.

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Abstract

The utility model belongs to the technical field of adipic acid production equipment, and particularly relates to a coarse adipic acid crystallization point detection system which comprises a crystallization point detection tank, a coarse adipic acid solution storage tank, a coarse adipic acid solution delivery pump, a feeding three-way control electromagnetic valve, a cooling water recovery tank and a crystallization point automatic detection time sequence controller, the crystallization point automatic detection time sequence controller is provided with a main signal connecting line; a thermometer is arranged outside the crystallization point detection tank; an electrode type liquid level alarm controller is also arranged at the top end of the crystallization point detection tank; a first discharge pipe is arranged at the bottom end of the crystallization point detection tank. According to the system disclosed by the utility model, the structure of the crystallization point detection tank is improved, and the automatic feeding detection time sequence is optimized, so that the continuous automatic detection and recording of the crystallization point of the crude adipic acid are realized, reliable data support is provided for the production and purification operation of the crude adipic acid, and the stable operation of the device is ensured.
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Description

TECHNICAL FIELD

[0001] The utility model belongs to adipic acid production equipment technical field, concretely relates to a detection system of crude adipic acid crystallization point. BACKGROUND

[0002] Oxidation reaction procedure is the core procedure in adipic acid production process, and the crude adipic acid generated in the oxidation reaction procedure is obtained after purification and drying, and the parameter of the sold product is qualified.Crystallization point is an important control parameter of oxidation procedure, and is the main basis for adjusting raw material ratio, which can represent whether the reaction procedure is normal on one hand, and provides necessary basis for controlling the temperature and vacuum state of each chamber of crystallizer in the refining and purification procedure on the other hand, so the detection work of crystallization point must be accurate and reliable.

[0003] Therefore, the utility model provides a detection system of crude adipic acid crystallization point, which determines the crystallization point of crude adipic acid by adopting automatic feeding continuous detection, so as to determine the concentration of crude adipic acid solution and ensure the quality of refined adipic acid product. UTILITY MODEL CONTENT

[0004] In order to solve the above technical problems, the application provides a detection system of crude adipic acid crystallization point, which is practical and reliable, and can solve the technical problems of poor continuity of the original detection system, on-site nitrous gas dispersion, material easy to emerge, large detection data error and high utility engineering loss. The system improves the structure of the crystallization point detection tank and optimizes the automatic feeding detection timing, realizes the continuous automatic detection and recording of the crystallization point of crude adipic acid, provides reliable data support for the production and purification operation of crude adipic acid, and ensures the stable operation of the device.

[0005] In order to realize the above technical purpose, the utility model adopts the following technical scheme:

[0006] A detection system of crude adipic acid crystallization point, comprising a crystallization point detection tank, a crude adipic acid solution storage tank, a crude adipic acid solution delivery pump, a feeding tee control solenoid valve, a cooling water recovery tank and a crystallization point automatic detection timing controller.

[0007] The crystallization point automatic detection timing controller is provided with a main signal connection line;

[0008] The crystallization point detection tank is externally provided with a thermometer;

[0009] The crystallization point detection tank is further provided with an electrode type liquid level alarm controller at the top end;

[0010] The crystallization point detection tank is provided with a first discharge pipe at the bottom end; the output end of the first discharge pipe is connected with the crude adipic acid solution storage tank in communication;

[0011] The crystallization point detection tank is provided with a detection tank jacket outside the tank, the detection tank jacket is hollow, and the detection tank jacket is connected in communication with an external cooling water inlet system through a cooling liquid inlet pipe;

[0012] The cooling liquid inlet pipe is also provided with a low-pressure steam inlet pipe connected in communication with an external low-pressure steam system.

[0013] The crystallization point detection tank is provided with an overflow port at the upper portion of the tank, and the overflow port is connected with a high-low overflow pipeline.

[0014] The detection tank jacket is also provided with a jacket cooling water return pipeline at the top end of the jacket, and the output end of the jacket cooling water return pipeline is connected in communication with a cooling water recovery tank.

[0015] The bottom end of the jacket is also provided with a second discharge pipe, and the output end of the second discharge pipe is discharged to a ditch.

[0016] The bottom end of the crude adipic acid solution storage tank is provided with a crude adipic acid storage tank discharge pipe, and the crude adipic acid solution storage tank is connected in communication with the inlet end of a crude adipic acid solution delivery pump through the crude adipic acid storage tank discharge pipe.

[0017] The output end of the crude adipic acid solution delivery pump is connected in communication with the inlet end of a feed three-way control electromagnetic valve through a crude adipic acid solution delivery pump discharge pipe.

[0018] The feed three-way control electromagnetic valve is provided with two outlet ends, namely a first outlet end and a second outlet end, the first outlet end of the feed three-way control electromagnetic valve is connected in communication with the high-low overflow pipeline through a pipeline, and the second outlet end of the feed three-way control electromagnetic valve is connected in communication with the crystallization point detection tank through a feed pipeline.

[0019] Further, an impeller type stirring paddle is installed inside the crystallization point detection tank, the stirring shaft of the impeller type stirring paddle extends from the top of the crystallization point detection tank, and the stirring shaft is connected with a stirring motor.

[0020] Further, the first discharge pipe is provided with a complete discharge valve.

[0021] Further, the temperature sensing end of the thermometer extends into the crystallization point detection tank, and the thermometer is provided with a temperature signal output end, the temperature signal output end is electrically connected with the main signal connection line of the crystallization point automatic detection time sequence controller through a first signal output line.

[0022] Further, the electrode type liquid level alarm controller is provided with a liquid level signal output end, and the liquid level signal output end is electrically connected with the main signal connection line of the crystallization point automatic detection time sequence controller through a second signal output line.

[0023] Further, the cooling liquid inlet pipe is provided with a cooling water inlet control valve at the connection with the external cooling water inlet system, the cooling water inlet control valve is an electromagnetic control valve, the cooling water inlet control valve is provided with a water inlet signal output end, and the water inlet signal output end is electrically connected with the main signal connection line of the crystallization point automatic detection time sequence controller through a third signal output line.

[0024] Further, the low-pressure steam inlet pipe is provided with a low-pressure steam inlet control valve at the connection with the external low-pressure steam system, the low-pressure steam inlet control valve is an electromagnetic control valve, the low-pressure steam inlet control valve is provided with a steam inlet signal output end, and the steam inlet signal output end is electrically connected with the main signal connection line of the crystallization point automatic detection time sequence controller through a fourth signal output line.

[0025] Further, the jacket cooling water return pipe is provided with a jacket cooling water return control valve, the jacket cooling water return control valve is an electromagnetic control valve, the jacket cooling water return control valve is provided with a water return signal output end, and the water return signal output end is electrically connected with the main signal connection line of the crystallization point automatic detection time sequence controller through a fifth signal output line.

[0026] Further, the output end of the high-low overflow pipeline is connected with the first discharge pipe; when the liquid material in the crystallization point detection tank is too much, the liquid material can be discharged through the overflow port and returned to the crude adipic acid solution storage tank.

[0027] Further, the top end of the crystallization point detection tank is further provided with a gas phase pipeline, the output end of the gas phase pipeline is connected with the external nitrous gas recovery system, and the gas phase pipeline is provided with a nitrous gas discharge valve.

[0028] The high-low overflow pipeline is connected with the crude adipic acid solution storage tank, and the gas phase pipeline is connected with the inlet of the nitrous gas recovery system, so that the micro-negative pressure in the crystallization point detection tank is controlled.

[0029] Further, the second discharge pipe is provided with a steam condensate discharge control valve, the steam condensate discharge control valve is provided with a condensate signal output end, and the condensate signal output end is electrically connected with the main signal connection line of the crystallization point automatic detection time sequence controller through a sixth signal output line.

[0030] Further, the crude adipic acid storage tank discharge pipe is provided with a crude adipic acid discharge valve.

[0031] Further, the crude adipic acid solution delivery pump discharge pipe is provided with a first manual valve.

[0032] Further, the feed three-way control electromagnetic valve is provided with a three-way control signal output end, and the three-way control signal output end is electrically connected with the main signal connection line of the crystallization point automatic detection time sequence controller through a seventh signal output line.

[0033] Further, the crystallization point automatic detection timing controller can adopt the conventional timing controller in the prior art, for example, ACTD-800 hot runner timing controller, heating runner MD18 temperature control hot runner card mold timing controller, ASCO timing controller E909 series and the like, and the structure is not the point of the application, so it will not be repeated.

[0034] Compared with the prior art, the utility model has the advantages of:

[0035] 1. The utility model realizes the continuous and stable detection of the crystallization point of the crude adipic acid solution in the adipic acid production, provides reliable data basis for the setting of the control parameters of the raw material ratio and the crystallizer in the crude adipic acid production process, and guarantees the high quality of the refined adipic acid product to a certain extent.

[0036] 2. The detection system of the crystallization point of the crude adipic acid is stable in operation, reliable in data and strong in continuity. After improving the original crystallization point detection system, the problems of nitrous gas dispersion, high utility engineering loss, easy material outburst and large detection data error in the operation process of the original system are solved, and the long-period stable operation of the device is realized. BRIEF DESCRIPTION OF DRAWINGS

[0037] Figure 1 It is the structural schematic diagram of the detection system of the crystallization point of the crude adipic acid in example 1.

[0038] In the drawing: 1, jacket cooling water return control valve, 2, jacket cooling water return pipeline, 3, gas phase pipeline, 4, electrode type liquid level alarm controller, 5, high and low overflow pipeline, 6, thermometer, 7, feed three-way control electromagnetic valve, 8, feed pipeline, 9, crude adipic acid solution conveying pump, 10, crude adipic acid solution storage tank, 11, crystallization point automatic detection timing controller, 12, cooling water inlet control valve, 13, steam condensate discharge control valve, 14, low-pressure steam inlet control valve, 15, crystallization point detection tank, 16, cooling liquid inlet pipe, 17, second discharge pipe, 18, first discharge pipe, 19, exhaust valve, 20, cooling water recovery tank, 31, nitrous gas discharge valve, 91, crude adipic acid storage tank discharge pipe, 92, crude adipic acid solution conveying pump discharge pipe, 93, first manual valve, 94, crude adipic acid discharge valve, 111, main signal connection line, 112, first signal output line, 113, second signal output line, 114, third signal output line, 115, fourth signal output line, 116, fifth signal output line, 117, sixth signal output line, 118, seventh signal output line. DETAILED DESCRIPTION

[0039] The utility model will be further described below in combination with the embodiments and drawings, but is not limited to the utility model.

[0040] In the description of the utility model, it needs to be explained that for the orientation words, if the orientation and position relationship indicated by the terms "upper", "lower", "top", "bottom", "inner", "outer" and the like is based on the orientation or position relationship shown in the drawings, it is only for the convenience of describing the utility model and simplifying the description, and does not indicate or imply that the device or element indicated must have a specific orientation, be constructed and operated in a specific orientation, and cannot be understood as limiting the specific protection scope of the utility model.

[0041] It needs to be explained that the terms "first", "second", "third", "1#", "2#" and the like in the specification and claims of the present application are used to distinguish similar objects, and do not have to be used to describe a specific order or sequence. It should be understood that the data used in this way can be interchanged under appropriate circumstances, so as to describe the embodiments of the present application described herein.

[0042] Embodiment 1

[0043] As Figure 1 shown, a crude adipic acid crystallization point detection system, including crystallization point detection tank 15, crude adipic acid solution storage tank 10, crude adipic acid solution delivery pump 9, feed three-way control solenoid valve 7, cooling water recovery tank 20 and crystallization point automatic detection timing controller 11;

[0044] The impeller type stirring paddle is installed in the crystallization point detection tank 15, the stirring shaft of the impeller type stirring paddle extends from the top of the crystallization point detection tank 15, and the stirring shaft is connected with a stirring motor;

[0045] The crystallization point automatic detection timing controller 11 is provided with a main signal connection line 111;

[0046] The crystallization point detection tank 15 is externally provided with a thermometer 6, the temperature sensing end of the thermometer 6 extends into the crystallization point detection tank 15, and the thermometer 6 is provided with a temperature signal output end, the temperature signal output end is electrically connected with the main signal connection line 111 of the crystallization point automatic detection timing controller 11 through a first signal output line 112;

[0047] The crystallization point detection tank 15 is further provided with an electrode type liquid level alarm controller 4 at the top end, the electrode type liquid level alarm controller 4 is provided with a liquid level signal output end, and the liquid level signal output end is electrically connected with the main signal connection line 111 of the crystallization point automatic detection timing controller 11 through a second signal output line 113;

[0048] The bottom end of the crystallization point detection tank 15 is provided with a first discharge pipe 18, and the first discharge pipe 18 is provided with a discharge valve 19;The output end of the first discharge pipe 18 is communicated with the crude adipic acid solution storage tank 10.

[0049] The crystallization point detection tank 15 is provided with a detection tank jacket outside, the detection tank jacket is hollow, and the detection tank jacket is connected with an external cooling water inlet system in communication through a cooling liquid inlet pipe 16; the cooling liquid inlet pipe 16 is provided with a cooling water inlet control valve 12 at the connection position with the external cooling water inlet system; the cooling water inlet control valve 12 is an electromagnetic control valve; the cooling water inlet control valve 12 is provided with a water inlet signal output end; and the water inlet signal output end is electrically connected with a main signal connection line 111 of a crystallization point automatic detection time sequence controller 11 through a third signal output line 114.

[0050] The cooling liquid inlet pipe 16 is also provided with a low-pressure steam inlet pipe (not marked in the figure); the low-pressure steam inlet pipe is connected with an external low-pressure steam system in communication; the low-pressure steam inlet pipe is provided with a low-pressure steam inlet control valve 14 at the connection position with the external low-pressure steam system; the low-pressure steam inlet control valve 14 is an electromagnetic control valve; the low-pressure steam inlet control valve 14 is provided with a steam inlet signal output end; and the steam inlet signal output end is electrically connected with the main signal connection line 111 of the crystallization point automatic detection time sequence controller 11 through a fourth signal output line 115.

[0051] The crystallization point detection tank 15 is provided with a detection tank jacket outside, the detection tank jacket is hollow, and the detection tank jacket is connected with an external cooling water inlet system in communication through a cooling liquid inlet pipe 16; the cooling liquid inlet pipe 16 is provided with a cooling water inlet control valve 12 at the connection position with the external cooling water inlet system; the cooling water inlet control valve 12 is an electromagnetic control valve; the cooling water inlet control valve 12 is provided with a water inlet signal output end; and the water inlet signal output end is electrically connected with a main signal connection line 111 of a crystallization point automatic detection time sequence controller 11 through a third signal output line 114.

[0052] The detection tank jacket is also provided with a jacket cooling water return pipe line 2 at the top end; the output end of the jacket cooling water return pipe line 2 is connected with a cooling water recovery tank 20 in communication; the jacket cooling water return pipe line 2 is provided with a jacket cooling water return control valve 1; the jacket cooling water return control valve 1 is an electromagnetic control valve; the jacket cooling water return control valve 1 is provided with a water return signal output end; and the water return signal output end is electrically connected with the main signal connection line 111 of the crystallization point automatic detection time sequence controller 11 through a fifth signal output line 116.

[0053] The crystallization point detection tank 15 is provided with a detection tank jacket outside, the detection tank jacket is hollow, and the detection tank jacket is connected with an external cooling water inlet system in communication through a cooling liquid inlet pipe 16; the cooling liquid inlet pipe 16 is provided with a cooling water inlet control valve 12 at the connection position with the external cooling water inlet system; the cooling water inlet control valve 12 is an electromagnetic control valve; the cooling water inlet control valve 12 is provided with a water inlet signal output end; and the water inlet signal output end is electrically connected with a main signal connection line 111 of a crystallization point automatic detection time sequence controller 11 through a third signal output line 114.

[0054] The crystallization point detection tank 15 is provided with a detection tank jacket outside, the detection tank jacket is hollow, and the detection tank jacket is connected with an external cooling water inlet system in communication through a cooling liquid inlet pipe 16; the cooling liquid inlet pipe 16 is provided with a cooling water inlet control valve 12 at the connection position with the external cooling water inlet system; the cooling water inlet control valve 12 is an electromagnetic control valve; the cooling water inlet control valve 12 is provided with a water inlet signal output end; and the water inlet signal output end is electrically connected with a main signal connection line 111 of a crystallization point automatic detection time sequence controller 11 through a third signal output line 114.

[0055] In addition, the high-low overflow pipe line 5 is connected with the crude adipic acid solution storage tank 10, and the gas phase pipe line 3 is connected with the nitrous gas recovery system inlet, so that the crystallization point detection tank 15 is kept in a micro-negative pressure state.

[0056] The jacket bottom end is further provided with a second discharge pipe 17, the output end of the second discharge pipe 17 is externally discharged into a ditch, the second discharge pipe 17 is provided with a steam condensate discharge control valve 13; the steam condensate discharge control valve 13 is provided with a condensate signal output end, the condensate signal output end is electrically connected with the main signal connection line 111 of the crystallization point automatic detection time sequence controller 11 through a sixth signal output line 117.

[0057] The bottom end of the crude adipic acid solution storage tank 10 is provided with a crude adipic acid storage tank discharge pipe 91, the crude adipic acid storage tank discharge pipe 91 is provided with a crude adipic acid discharge valve 94, and the crude adipic acid solution storage tank 10 is connected with the inlet end of the crude adipic acid solution conveying pump 9 through the crude adipic acid storage tank discharge pipe 91.

[0058] The output end of the crude adipic acid solution conveying pump 9 is connected with the inlet end of the feed three-way control electromagnetic valve 7 through a crude adipic acid solution conveying pump discharge pipe 92, and the crude adipic acid solution conveying pump discharge pipe 92 is provided with a first manual valve 93.

[0059] The feed three-way control electromagnetic valve 7 is provided with two outlet ends, namely a first outlet end and a second outlet end, the first outlet end of the feed three-way control electromagnetic valve 7 is connected with the high-low position overflow pipeline 5 through a pipeline, and the second outlet end of the feed three-way control electromagnetic valve 7 is connected with the middle part of the crystallization point detection tank 15 through a feed pipeline 8.

[0060] The feed three-way control electromagnetic valve 7 is provided with a three-way control signal output end, and the three-way control signal output end is electrically connected with the main signal connection line 111 of the crystallization point automatic detection time sequence controller 11 through a seventh signal output line 118.

[0061] The crystallization point automatic detection time sequence controller 11 can adopt a conventional time sequence controller in the prior art, for example, an ACTD-800 hot runner time sequence controller, a heating runner MD18 temperature control hot runner mold clamping time sequence controller and an ASCO time sequence controller E909 series of equipment, and the structure is not the point of the application, so it will not be repeated here.

[0062] The temperature signal output end of the thermometer 6 is electrically connected with the main signal connecting line 111 of the crystallization point automatic detection time sequence controller 11 through the first signal output line 112, the liquid level signal output end of the electrode type liquid level alarm controller 4 is electrically connected with the main signal connecting line 111 of the crystallization point automatic detection time sequence controller 11 through the second signal output line 113, the water inlet signal output end of the cooling water inlet control valve 12 is electrically connected with the main signal connecting line 111 of the crystallization point automatic detection time sequence controller 11 through the third signal output line 114, the steam inlet signal output end of the low-pressure steam inlet control valve 14 is electrically connected with the main signal connecting line 111 of the crystallization point automatic detection time sequence controller 11 through the fourth signal output line 115, the water return signal output end of the jacket cooling water return control valve 1 is electrically connected with the main signal connecting line 111 of the crystallization point automatic detection time sequence controller 11 through the fifth signal output line 116, the condensate signal output end of the steam condensate discharge control valve 13 is electrically connected with the main signal connecting line 111 of the crystallization point automatic detection time sequence controller 11 through the sixth signal output line 117, and the three-way control signal output end of the feed three-way control electromagnetic valve 7 is electrically connected with the main signal connecting line 111 of the crystallization point automatic detection time sequence controller 11 through the seventh signal output line 118, which all adopt the conventional means in the prior art.

[0063] The thermometer 6, the cooling water inlet control valve 12, the low-pressure steam inlet control valve 14, the jacket cooling water return control valve 1, the steam condensate discharge control valve 13 and the feed three-way control electromagnetic valve 7 all adopt the conventional models of equipment in the prior art, and the structures are not the points of the present application, so the description is not repeated.

[0064] The control mode of the crystallization point automatic detection time sequence controller 11 on the thermometer 6, the electrode type liquid level alarm controller 4, the cooling water inlet control valve 12, the low-pressure steam inlet control valve 14, the jacket cooling water return control valve 1, the steam condensate discharge control valve 13 and the feed three-way control electromagnetic valve 7 can adopt the conventional setting in the prior art, and is not the point of the present application, so the description is not repeated.

[0065] The crystallization point automatic detection time sequence controller 11 can set detection steps in time sequence, heat and cool the detection solution to obtain the temperature change curve, and obtain the crystallization point of the detection solution according to the slope change characteristics.

[0066] The present application realizes continuous and stable detection of the crystallization point of the crude adipic acid solution in the production of adipic acid, provides reliable data basis for the setting of the control parameters of the raw material ratio and the crystallizer in the production process of the crude adipic acid, and guarantees the high quality of the refined adipic acid product to a certain extent.

[0067] The detection process of the detection system of the crude adipic acid crystallization point is as follows:

[0068] (1) Liquid filling process: before the system is operated, the feed three-way control electromagnetic valve 7, the exhaust valve 19, the cooling water inlet control valve 12, the low-pressure steam inlet control valve 14, the jacket cooling water return control valve 1, the nitrous gas exhaust valve 31, the crude adipic acid exhaust valve 94, and the first manual valve 93 are all set to the closed state.

[0069] When operated, first, the crude adipic acid exhaust valve 94, the crude adipic acid solution conveying pump 9, and the first manual valve 93 are opened, the crude adipic acid solution in the crude adipic acid solution storage tank 10 is discharged, and the crude adipic acid solution is pumped into the feed three-way control electromagnetic valve 7 by the crude adipic acid solution conveying pump 9, then the feed three-way control electromagnetic valve 7 is opened, and the discharge is set to pass through the second outlet end, then through the feed pipeline 8, the feeding to the crystallization point detection tank 15 is started, the three-way control electromagnetic valve 7 opening time and the second outlet end discharge time of the three-way control electromagnetic valve 7 are regulated by setting the crystallization point automatic detection time sequence controller 11, the time control is 18 minutes, and the feeding is stopped after the set time is reached.

[0070] During the liquid filling process, the state of the electrode type liquid level alarm controller 4 is detected, if alarm, the electrode type liquid level alarm controller 4 sends a stop signal to the crystallization point automatic detection time sequence controller 11, and the crystallization point automatic detection time sequence controller 11 stops the detection time sequence, and after the alarm is eliminated and reset, the time sequence can continue to operate.

[0071] Then, the second outlet end of the feed three-way control electromagnetic valve 7 is closed and the first outlet end of the feed three-way control electromagnetic valve 7 is opened by the crystallization point automatic detection time sequence controller 11, the discharge of the feed three-way control electromagnetic valve 7 is diverted to the crude adipic acid solution storage tank 10, and the circulation is carried out to prevent the crude adipic acid solution conveying pump 9 from being pressure-stopped.

[0072] (2) Heating process: the low-pressure steam inlet control valve 14 and the steam condensate discharge control valve 13 are controlled to be opened by the crystallization point automatic detection time sequence controller 11, the steam is introduced into the detection tank jacket through the externally connected low-pressure steam system to heat the crystallization point detection tank 15, the opening time of the low-pressure steam inlet control valve 14 and the steam condensate discharge control valve 13 is regulated by the crystallization point automatic detection time sequence controller 11, the time control is 2 minutes, the low-pressure steam inlet control valve 14 and the steam condensate discharge control valve 13 are closed after the set time is reached; a small amount of nitrous gas is generated in this process, at this time, the nitrous gas is discharged and recovered to the subsequent process through the gas phase pipeline 3 by opening the nitrous gas exhaust valve 31.

[0073] (3) cooling crystallization process: through the crystallization point automatic detection time sequence controller 11 control open cooling water inlet control valve 12 and jacket cooling water backwater control valve 1, through the crystallization point automatic detection time sequence controller 11 control closing low pressure steam inlet control valve 14 and steam condensate discharge control valve 13, through the cooling water inlet system to the detection tank jacket into high purity cooling water, the detection material in the crystallization point detection tank 15 is cooled, the heat exchange high purity water is recycled through the cooling water backwater pipeline 2, reduces the loss of high purity water;In the crystallization point detection tank 15, the detection liquid is cooled due to the decrease of solubility, adipic acid is gradually crystallized.

[0074] (4) the generation of crystallization point: in the above cooling crystallization process, the temperature of the detection liquid in the crystallization point detection tank 15 is detected and recorded by the thermometer 6, and the temperature curve is obtained;The temperature curve slope is analyzed according to the principle of crystallization latent heat release in the material crystallization process by computer, and the crystallization point is automatically generated.

[0075] The temperature of the solution in the crystallization point detection tank 15 is detected by the thermometer 6, if the alarm, the thermometer 6 sends a stop signal to the crystallization point automatic detection time sequence controller 11, and the crystallization point automatic detection time sequence controller 11 stops the detection time sequence, and the time sequence can continue to run after the alarm is reset.

[0076] The crystallization detection cycle of the crude adipic acid crystallization point detection system is about 25-35 minutes, preferably 30 minutes, and the liquid filling time can be adjusted according to the actual working condition, the liquid filling time is related to the volume of the crystallization point detection tank 15, the volume of the crystallization point detection tank 15 is large, the liquid volume is large, and the required time can be prolonged.

[0077] After the crystallization point is generated, the crystallization point automatic detection time sequence controller 11 will automatically perform the next round of detection, enter the next round of liquid filling process, open the feed three-way control electromagnetic valve 7, and set the discharge through the second outlet end, feed the crystallization point detection tank 15, and also can replace the previous detection liquid into the crude adipic acid solution storage tank 10 through the high-low overflow pipeline 5, realize the replacement of the detection liquid.

[0078] The crude adipic acid crystallization point detection system has stable operation, reliable data and strong continuity in operation. Through the improvement of the original crystallization point detection system, the problems of nitrous gas dispersion, high utility consumption, material easy to escape and large detection data error in the operation process of the original system are solved, and the long period stable operation of the device is realized.

[0079] The above embodiment is an example of the embodiment of the present application, and the embodiment of the present application is not limited by the above embodiment, and any change, modification, replacement, combination, simplification, which does not deviate from the spirit and principle of the present application, should be an equivalent replacement mode, and all are included in the protection scope of the present application.

Claims

1. A system for detecting the crystallization point of crude adipic acid, characterized in that it comprises: It includes a crystallization point detection tank, a crude adipic acid solution storage tank, a crude adipic acid solution transfer pump, a feed three-way control solenoid valve, a cooling water recovery tank, and an automatic crystallization point detection timing controller; The automatic crystallization point detection timing controller is equipped with a main signal connection line; A thermometer is installed outside the crystallization point detection tank; The top of the crystallization point detection tank is also equipped with an electrode-type liquid level alarm controller. The bottom of the crystallization point detection tank is provided with a first discharge pipe; the output end of the first discharge pipe is connected to the crude adipic acid solution storage tank. The crystallization point detection tank is provided with a detection tank jacket on its outer periphery. The detection tank jacket is hollow and is connected to an external cooling water inlet system through a coolant inlet pipe. The coolant inlet pipe is also equipped with a low-pressure steam inlet pipe, which is connected to an external low-pressure steam system. The crystallization point detection tank is provided with an overflow port at the top, and the overflow port is connected to high and low level overflow pipelines; The top of the jacket of the detection tank is also provided with a jacket cooling water return pipeline, and the output end of the jacket cooling water return pipeline is connected to the cooling water recovery tank. The jacket is also provided with a second discharge pipe at the bottom end, and the output end of the second discharge pipe is discharged into the trench. The bottom of the crude adipic acid solution storage tank is equipped with a crude adipic acid storage tank discharge pipe, and the crude adipic acid solution storage tank is connected to the inlet end of the crude adipic acid solution transfer pump through the crude adipic acid storage tank discharge pipe. The output end of the crude adipic acid solution transfer pump is connected to the inlet end of the feed tee control solenoid valve through the discharge pipe of the crude adipic acid solution transfer pump. The feed three-way control solenoid valve has two outlet ends, namely the first outlet end and the second outlet end. The first outlet end of the feed three-way control solenoid valve is connected to the high and low level overflow pipeline through a pipeline, and the second outlet end of the feed three-way control solenoid valve is connected to the crystallization point detection tank through the feed pipeline.

2. The coarse adipic acid crystallization point detection system of claim 1, wherein, The temperature sensing end of the thermometer extends into the crystallization point detection tank, and the thermometer is equipped with a temperature signal output end. The temperature signal output end is electrically connected to the main signal connection line of the automatic crystallization point detection timing controller through the first signal output line.

3. The coarse adipic acid crystallization point detection system of claim 1, wherein, The electrode-type liquid level alarm controller is equipped with a liquid level signal output terminal, which is electrically connected to the main signal connection line of the crystallization point automatic detection timing controller through a second signal output line.

4. The coarse adipic acid crystallization point detection system of claim 1, wherein, A cooling water inlet control valve is provided at the connection between the coolant inlet pipe and the external cooling water inlet system. The cooling water inlet control valve is an electromagnetic control valve and has an inlet signal output terminal. The inlet signal output terminal is electrically connected to the main signal connection line of the crystallization point automatic detection timing controller through a third signal output line.

5. The coarse adipic acid crystallization point detection system of claim 1 wherein, A low-pressure steam inlet control valve is provided at the connection between the low-pressure steam inlet pipe and the external low-pressure steam system. The low-pressure steam inlet control valve is an electromagnetic control valve and has an inlet steam signal output terminal. The inlet steam signal output terminal is electrically connected to the main signal connection line of the crystallization point automatic detection timing controller through the fourth signal output line.

6. The coarse adipic acid crystallization point detection system of claim 1 wherein, The jacket cooling water return pipeline is provided with a jacket cooling water return control valve, which is an electromagnetic control valve.

7. The coarse adipic acid crystallization point detection system of claim 1 wherein, The output end of the high-low position overflow pipeline is connected with the first discharge pipe.

8. The coarse adipic acid crystallization point detection system of claim 1, wherein, The top end of the crystallization point detection tank is further provided with a gas phase pipeline, the output end of which is connected with an externally connected nitrous gas recovery system; the gas phase pipeline is provided with a nitrous gas discharge valve.

9. The coarse adipic acid crystallization point detection system of claim 1 wherein, The second discharge pipe is provided with a steam condensate discharge control valve; the steam condensate discharge control valve is provided with a condensate signal output end, which is electrically connected with the main signal connection line of the crystallization point automatic detection time sequence controller through a sixth signal output line.

10. The coarse adipic acid crystallization point detection system of claim 1, wherein, The feed three-way control electromagnetic valve is provided with a three-way control signal output end, which is electrically connected with the main signal connection line of the crystallization point automatic detection time sequence controller through a seventh signal output line.