Hexamethylene diammonium adipate solution sample recycling system

Abstract

The utility model belongs to chemical equipment technical field, concretely relates to adipic acid hexamethylene diamine salt solution sample recycling system. Including pretreatment jar, the discharge port of pretreatment jar is connected to the feed inlet of purification tank through metering pump, the discharge port of purification tank is connected to reactor and temporary storage jar respectively through first switch valve, the discharge port of temporary storage jar is connected to reactor and waste liquid treatment unit respectively through second switch valve, is equipped with first on -line concentration meter in the purification tank, is equipped with second on -line concentration meter in reactor, is equipped with laser turbidimeter in temporary storage jar;Pretreatment jar and purification tank are connected with desalted water storage jar respectively;The displacement system is connected to the purification tank, the agitator and the adsorption layer are equipped in the purification tank, and the discharge outlet pipeline of the purification tank is equipped with fiber spectrum appearance;Still including PLC control system. Through the closed loop recovery system of construction, the efficient resource utilization of sample and the classification reuse of cleaning water are realized, the raw material loss and wastewater discharge are reduced, and the recovery efficiency is optimized.

Description

Technical Field

[0001] This utility model belongs to the field of chemical equipment technology, specifically relating to a system for recycling adipic acid hexamethylenediamine salt solution samples. Background Technology

[0002] In the production process of hexamethylenediamine adipic acid salt solution, high-frequency sampling and testing of intermediate and finished products are required to monitor key indicators such as concentration and purity. Direct discharge of these samples after testing not only wastes raw materials but also increases the wastewater treatment load. Traditional treatment methods often involve simple collection followed by direct return to the reaction system, lacking targeted purification processes. This results in trace impurities and residual substances carried in the samples entering the main reaction system, affecting the stability of the final product quality. Simultaneously, the lack of effective isolation and protection measures during the recovery process allows the solution to easily oxidize upon contact with air, leading to increased color and further deterioration of product performance. Furthermore, traditional recovery processes often involve direct discharge of washing water without graded reuse, resulting in low water resource utilization. The lack of real-time monitoring of the concentration and cleanliness of recovered materials necessitates frequent manual sampling and testing, which is cumbersome, prone to human error, and fails to meet the stability and economic requirements of continuous production. Utility Model Content

[0003] In view of the shortcomings of the prior art, the purpose of this utility model is to provide a sample recycling system for adipic acid hexamethylenediamine salt solution. By constructing a closed-loop recycling system, the system realizes efficient resource utilization of the sample and graded reuse of washing water, reducing raw material loss and wastewater discharge. Through fully automated control, the system inhibits oxidation and deterioration, ensures color value stability, and optimizes recycling efficiency.

[0004] This utility model is achieved using the following technical solution:

[0005] The adipic acid hexamethylenediamine salt solution sample recycling system includes a pretreatment tank, the outlet of which is connected to the inlet of a purification tank via a metering pump. The outlet of the purification tank is connected to a reactor and a temporary storage tank via a first switching valve. The outlet of the temporary storage tank is connected to a reactor and a waste liquid treatment unit via a second switching valve. A first online concentration meter is installed in the purification tank, a second online concentration meter is installed in the reactor, and a laser turbidimeter is installed in the temporary storage tank. The pretreatment tank and the purification tank are connected to a demineralized water storage tank. The purification tank is connected to a displacement system, and its top exhaust pipe is connected to a waste gas absorption tower. The purification tank contains a stirrer and an adsorption layer. A fiber optic spectrometer is installed on the outlet pipe of the purification tank. The system also includes a PLC control system.

[0006] The feed inlet of the pretreatment tank is equipped with a removable filter screen.

[0007] The outlet pipeline of the demineralized water storage tank is provided with two branches in parallel. One branch is connected to the feed inlet of the pretreatment tank through a high-pressure cleaning pump; the other branch is connected to the feed inlet of the purification tank through a demineralized water control valve. The high-pressure cleaning pump and the demineralized water control valve are electrically connected to the PLC control system.

[0008] The demineralized water storage tank and the purification tank are each equipped with a temperature sensor inside, and both the demineralized water storage tank and the purification tank are equipped with an electric heat tracing assembly on their outer walls. The temperature sensor and the electric heat tracing assembly are electrically connected to the PLC control system.

[0009] The replacement system includes a nitrogen pipeline, a nitrogen control valve on the nitrogen pipeline, and a trace oxygen sensor installed inside the purification tank; the exhaust pipeline is equipped with an exhaust valve, and the nitrogen control valve, the exhaust valve, and the trace oxygen sensor are electrically connected to the PLC control system.

[0010] The first switching valve, the second switching valve, the first online concentration meter, the second online concentration meter, the laser turbidimeter, and the fiber optic spectrometer are all electrically connected to the PLC control system.

[0011] The working principle of the adipic acid hexamethylenediamine salt solution sample recycling system is as follows:

[0012] The samples to be recovered after testing first enter the pretreatment tank. After large particulate impurities are removed by a detachable filter, they are precisely delivered to the purification tank by a metering pump. The purification tank is first purged with nitrogen through a nitrogen pipeline. The nitrogen control valve regulates the air intake, and the exhaust valve discharges the air-containing waste gas to the waste gas absorption tower until the oxygen content in the tank is detected by a trace oxygen sensor to drop to a preset value, ensuring that the solution does not oxidize or deteriorate during subsequent processing. According to the amount of material measured by the metering pump, the PLC control system opens the demineralized water control valve, adding a quantitative amount of demineralized water from the demineralized water storage tank to the purification tank. At the same time, the agitator is started to mix the material evenly. The solution concentration is monitored in real time by the first online concentration meter in the purification tank. Once the preset value is reached, the demineralized water control valve is closed. The electric heating component on the outer wall of the purification tank, together with the temperature sensor, heats the material in the tank to above 50°C to prevent crystallization. The material under agitation state further adsorbs fine impurities and pigments through the internal adsorption layer. The purified material enters the reactor through the first switching valve and mixes with the main solution in the reactor. After the material is discharged, the PLC control system starts the high-pressure cleaning pump, which sends the demineralized water heated to above 50°C by the electric heating component of the demineralized water storage tank into the pretreatment tank. The cleaning liquid flows through the purification tank and then into the reactor. During this process, the concentration of the main solution is monitored by the second online concentration meter in the reactor. When the concentration drops to the preset value, the first switching valve switches to the temporary storage tank passage, and the remaining cleaning water enters the temporary storage tank for temporary storage. After the cleaning process is completed, the high-pressure cleaning pump is turned off. The laser turbidimeter in the temporary storage tank detects the turbidity of the material. If the turbidity is lower than the preset value, this part of the material is reused in the reactor as demineralized water supplement in the next reaction through the second switching valve. If the turbidity exceeds the standard, it is discharged to the waste liquid treatment unit through the second switching valve. The fiber optic spectrometer on the outlet pipeline of the purification tank detects the color value of the material in real time. When the color value is higher than the preset value, it prompts to replace the adsorption layer in the purification tank to ensure the stability of the quality of the recovered material.

[0013] Compared with the prior art, the beneficial effects of this utility model are as follows:

[0014] The adipic acid hexamethylenediamine salt solution sample recycling system described in this invention achieves resource recovery and efficient reuse of samples after testing, significantly reducing raw material waste and wastewater discharge. Through a combination of staged filtration and adsorption purification, the purity of the recovered material is greatly improved, effectively preventing impurities from interfering with the main reaction system. Nitrogen replacement and a fully enclosed design fundamentally inhibit solution oxidation and deterioration, ensuring the color stability of the recovered material. Precise temperature control and anti-crystallization design ensure the fluidity of the material during the recovery process, avoiding pipeline blockage and other problems. Simultaneously, the system enables the staged reuse of cleaning water, significantly improving water resource utilization and reducing wastewater treatment pressure. The fully automated monitoring and linkage control mechanism reduces manual intervention, lowers operational errors, and improves production continuity and stability, achieving overall synergistic optimization of recovery efficiency, product quality, and production economy. Attached Figure Description

[0015] Figure 1 This is a schematic diagram of the adipic acid hexamethylenediamine salt solution sample recycling system of the present invention;

[0016] In the diagram: 1. Pretreatment tank; 2. Metering pump; 3. Purification tank; 4. First switching valve; 5. Reactor; 6. Temporary storage tank; 7. Second switching valve; 8. Waste liquid treatment unit; 9. First online concentration meter; 10. Second online concentration meter; 11. Laser turbidimeter; 12. Demineralized water storage tank; 13. Waste gas absorption tower; 14. Agitator; 15. Adsorption layer; 16. Fiber optic spectrometer; 17. Removable filter screen; 18. High-pressure cleaning pump; 19. Demineralized water control valve; 20. Temperature sensor; 21. Electric heating assembly; 22. Nitrogen control valve; 23. Micro oxygen sensor; 24. Exhaust valve. Detailed Implementation

[0017] To make the objectives and technical solutions of this utility model clearer, the present utility model will be further described in detail below with reference to the accompanying drawings.

[0018] Example 1

[0019] like Figure 1 As shown, the adipic acid hexamethylenediamine salt solution sample recycling system includes a pretreatment tank 1. The outlet of the pretreatment tank 1 is connected to the inlet of the purification tank 3 via a metering pump 2. The outlet of the purification tank 3 is connected to the reactor 5 and the temporary storage tank 6 via a first switching valve 4. The outlet of the temporary storage tank 6 is connected to the reactor 5 and the waste liquid treatment unit 8 via a second switching valve 7. The purification tank 3 is equipped with a first online concentration meter 9, the reactor 5 is equipped with a second online concentration meter 10, and the temporary storage tank 6 is equipped with a laser turbidimeter 11. The pretreatment tank 1 and the purification tank 3 are respectively connected to the demineralized water storage tank 12. The purification tank 3 is connected to a displacement system, and its top exhaust pipe is connected to the waste gas absorption tower 13. The purification tank 3 is equipped with a stirrer 14 and an adsorption layer 15. The outlet pipe of the purification tank 3 is equipped with a fiber optic spectrometer 16. The system also includes a PLC control system.

[0020] The feed inlet of the pretreatment tank 1 is equipped with a detachable filter screen 17.

[0021] The outlet pipeline of the demineralized water storage tank 12 is provided with two branches in parallel. One branch is connected to the inlet of the pretreatment tank 1 through the high-pressure cleaning pump 18; the other branch is connected to the inlet of the purification tank 3 through the demineralized water control valve 19. The high-pressure cleaning pump 18 and the demineralized water control valve 19 are electrically connected to the PLC control system.

[0022] Temperature sensors 20 are installed inside the demineralized water storage tank 12 and the purification tank 3 respectively. Electric heat tracing components 21 are installed on the outer walls of both the demineralized water storage tank 12 and the purification tank 3. The temperature sensors 20 and the electric heat tracing components 21 are electrically connected to the PLC control system respectively.

[0023] The replacement system includes a nitrogen pipeline, a nitrogen control valve 22 on the nitrogen pipeline, and a trace oxygen sensor 23 installed inside the purification tank 3; the exhaust pipeline is equipped with an exhaust valve 24, and the nitrogen control valve 22, the exhaust valve 24, and the trace oxygen sensor 23 are electrically connected to the PLC control system.

[0024] The first switching valve 4, the second switching valve 7, the first online concentration meter 9, the second online concentration meter 10, the laser turbidimeter 11, and the fiber optic spectrometer 16 are electrically connected to the PLC control system.

[0025] The specific steps for doing this are as follows:

[0026] The operator pours the tested adipic acid hexamethylenediamine salt solution sample into the pretreatment tank 1. After the sample is filtered through the removable filter screen 17 at the tank opening, it is transported to the purification tank 3 by the metering pump 2. After the transport is completed, the PLC control system opens the nitrogen control valve 22 and the exhaust valve 24 to introduce nitrogen into the purification tank 3 for replacement. The waste gas enters the waste gas absorption tower 13 for treatment through the exhaust valve 24. When the trace oxygen sensor 23 shows that the oxygen content in the purification tank 3 is ≤50ppm, the nitrogen control valve 22 and the exhaust valve 24 are closed to complete the replacement. Based on the material quantity feedback from metering pump 2, the PLC control system calculates the required amount of demineralized water and opens the demineralized water control valve 19. The demineralized water enters the purification tank 3 from the demineralized water storage tank 12. At the same time, the stirrer 14 is started, and the first online concentration meter 9 monitors the solution concentration in real time. When the concentration reaches 40 wt.%, the demineralized water control valve 19 is closed, and the electric heating component 21 of the purification tank 3 is started to heat the material temperature to 55°C and keep it stable. After the material is fully purified by the adsorption layer 15 under the action of stirring, the first switching valve 4 switches to the reactor 5 passage, and the purified material enters the reactor 5 to mix with the main solution. After the material transfer is completed, the PLC control system starts the high-pressure cleaning pump 18. The demineralized water preheated to 55°C in the demineralized water storage tank 12 is pressurized by the high-pressure cleaning pump 18 and enters the pretreatment tank 1. The pretreatment tank 1, purification tank 3 and related pipelines are flushed in sequence. The cleaning solution enters the reactor 5 through the first switching valve 4. During this period, the second online concentration meter 10 monitors the concentration of the solution in the reactor 5. When the concentration drops to 57 wt.%, the first switching valve 4 switches to the temporary storage tank 6 channel, and the remaining cleaning water flows into the temporary storage tank 6. After flushing for 15 minutes, the high-pressure cleaning pump 18 is turned off. The laser turbidimeter 11 in the temporary storage tank 6 detects the remaining liquid. If the turbidity is ≤1 NTU, the liquid is temporarily stored in the temporary storage tank 6 and will be transported to the reactor 5 for use as demineralized water in the next reaction through the second switching valve 7. If the turbidity is >1 NTU, it is discharged to the waste liquid treatment unit 8 through the second switching valve 7. Throughout the operation, the fiber optic spectrometer 16 at the outlet of the purification tank 3 continuously monitors the color value of the material. When the color value is ≥3APHA, the PLC control system issues a prompt signal, and the operator promptly replaces the adsorption layer 15 inside the purification tank 3 to ensure that the quality of the subsequently recovered material meets the requirements.

Claims

1. A system for recycling adipic acid hexamethylenediamine salt solution samples, characterized in that, The system includes a pretreatment tank (1), the outlet of which is connected to the inlet of the purification tank (3) via a metering pump (2), the outlet of the purification tank (3) via a first switching valve (4) to the reactor (5) and the temporary storage tank (6), the outlet of the temporary storage tank (6) via a second switching valve (7) to the reactor (5) and the waste liquid treatment unit (8), the purification tank (3) is equipped with a first online concentration meter (9), the reactor (5) is equipped with a second online concentration meter (10), and the temporary storage tank (6) is equipped with a laser turbidity meter (11); the pretreatment tank (1) and the purification tank (3) are respectively connected to the demineralized water storage tank (12); the purification tank (3) is connected to a displacement system, and its top exhaust pipe is connected to the waste gas absorption tower (13); the purification tank (3) is equipped with a stirrer (14) and an adsorption layer (15) inside, and a fiber optic spectrometer (16) is installed on the outlet pipe of the purification tank (3); and a PLC control system is also included.

2. The adipic acid hexamethylenediamine salt solution sample recycling system according to claim 1, characterized in that, The feed inlet of the pretreatment tank (1) is equipped with a removable filter screen (17).

3. The adipic acid hexamethylenediamine salt solution sample recycling system according to claim 1, characterized in that, Two branches are connected in parallel on the outlet pipeline of the demineralized water storage tank (12). One branch is connected to the feed inlet of the pretreatment tank (1) through a high-pressure cleaning pump (18); the other branch is connected to the feed inlet of the purification tank (3) through a demineralized water control valve (19). The high-pressure cleaning pump (18) and the demineralized water control valve (19) are electrically connected to the PLC control system respectively.

4. The adipic acid hexamethylenediamine salt solution sample recycling system according to claim 1, characterized in that, Temperature sensors (20) are installed inside the demineralized water storage tank (12) and the purification tank (3), and electric heat tracing components (21) are installed on the outer walls of the demineralized water storage tank (12) and the purification tank (3). The temperature sensors (20) and the electric heat tracing components (21) are electrically connected to the PLC control system.

5. The adipic acid hexamethylenediamine salt solution sample recycling system according to claim 4, characterized in that, The replacement system includes a nitrogen pipeline, a nitrogen control valve (22) on the nitrogen pipeline, and a trace oxygen sensor (23) installed inside the purification tank (3); the exhaust pipeline is equipped with an exhaust valve (24), and the nitrogen control valve (22), the exhaust valve (24), and the trace oxygen sensor (23) are electrically connected to the PLC control system.

6. The adipic acid hexamethylenediamine salt solution sample recycling system according to claim 1, characterized in that, The first switching valve (4), the second switching valve (7), the first online concentration meter (9), the second online concentration meter (10), the laser turbidity meter (11), and the fiber optic spectrometer (16) are electrically connected to the PLC control system.

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