Rectification column bottom material oil recovery device
By designing a distillation column bottom material oil and gas recovery device, gas-solid phase separation is achieved through vacuum heating and stirring, followed by condensation in a condenser. The organic matter recovery rate reaches 80%, solving the problem of the inability to separate and purify the residual liquid in the distillation column bottom, and realizing efficient recovery of raw materials and cost reduction.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- XINJIANG ZHONGTAI XINXIN CHEM TECH CO LTD
- Filing Date
- 2025-07-30
- Publication Date
- 2026-07-21
AI Technical Summary
In the current dichlorobenzene production process, the residue in the distillation column bottoms cannot be further separated and purified, leading to increased waste, raw material waste, and higher production costs.
A distillation column bottom material oil and gas recovery device was designed, including a residual liquid tank, an oil and gas recovery machine, a condenser, and a discharge buffer tank. The device uses heating and stirring under vacuum conditions, gas-solid phase separation by the oil and gas recovery machine, and condensation by the condenser to ultimately achieve the recovery and utilization of organic matter.
It effectively recovers more than 80% of organic matter, reduces waste generation, realizes waste reuse, and reduces production costs.
Smart Images
Figure CN224524007U_ABST
Abstract
Description
Technical Field
[0001] This utility model relates to the field of oil and gas recovery technology, and is a device for recovering oil and gas from the bottom material of a distillation column. Background Technology
[0002] Polyphenylene sulfide (PPS) is a novel high-performance thermoplastic resin with advantages such as high mechanical strength, high temperature resistance, chemical resistance, flame retardancy, good thermal stability, and excellent electrical properties. It has wide applications in the electronics, automotive, machinery, and chemical industries. There are many methods for synthesizing PPS, such as the self-condensation of halothiophenol salts, melt polymerization of p-halodiphenylene and sulfur, electrophilic reaction of sulfur and benzene, solution condensation of alkali metal sulfides with p-dihalobenzene (sodium sulfide method), solution condensation of sulfur and p-dichlorobenzene (sulfur solution method), and polymerization of diphenyl disulfide under Lewis acid conditions, etc.
[0003] Dichlorobenzene, the main raw material for the production of polyphenylene sulfide (PPS), is produced by adding ferric trichlorobenzene to dehydrated benzene. Chlorine gas is then passed through the benzene solution containing ferric trichloride to initiate the reaction. The reaction produces a mixture containing monochlorobenzene, para-dichlorobenzene, m-dichlorobenzene, o-dichlorobenzene, trichlorobenzene, and tetrachlorobenzene. After the reaction mixture passes through a distillation column, a measured amount of the heavy ferric trichloride-containing residue is discharged from the bottom of the column. This residue contains a large amount of organic matter and solids, making it unsuitable for subsequent distillation and purification; therefore, it must be treated as hazardous waste.
[0004] Therefore, it is necessary to research and invent a device for recovering oil and gas from the bottom of a distillation column. Summary of the Invention
[0005] This utility model provides a distillation column bottom material oil and gas recovery device, which overcomes the shortcomings of the above-mentioned prior art. It can effectively solve the problem that the bottom liquid in the existing dichlorobenzene production process cannot be further separated and purified, which increases the amount of waste generated, and thus causes raw material waste and increased production costs.
[0006] The technical solution of this utility model is achieved through the following measures: a distillation column bottom material oil and gas recovery device, including a residual liquid tank, an oil and gas recovery machine, a condenser, and a discharge buffer tank. The top inlet of the residual liquid tank is fixedly connected to a first material conveying pipeline. The bottom outlet of the residual liquid tank is fixedly connected to the first inlet at the top of the oil and gas recovery machine. The top outlet of the oil and gas recovery machine is fixedly connected to the top inlet of the condenser. The bottom outlet of the condenser is fixedly connected to the first inlet at the top of the discharge buffer tank. The lower outlet of the discharge buffer tank is fixedly connected to a fifth material conveying pipeline.
[0007] The following are further optimizations and / or improvements to the above-mentioned utility model technical solution:
[0008] The second and fifth material conveying pipelines are respectively equipped with residual liquid conveying pumps and discharge pumps.
[0009] The top outlet of the aforementioned discharge buffer tank is fixedly connected to a negative pressure extraction pipeline.
[0010] The aforementioned oil and gas recovery machine is equipped with an agitator inside and a jacket outside, with a heating component inside the jacket.
[0011] The bottom outlet of the aforementioned oil and gas recovery machine is fixedly connected to a discharge pipeline, the second inlet at the top of the oil and gas recovery machine is fixedly connected to a first nitrogen pipeline, and the upper outlet of the oil and gas recovery machine is fixedly connected to a first overflow pipeline.
[0012] The condenser has a cooling water supply line fixedly connected to its bottom inlet and a cooling water return line fixedly connected to its top outlet.
[0013] The aforementioned oil and gas recovery machine is fixedly equipped with a first pressure gauge and a first thermometer, and a second thermometer is fixedly installed on the second material conveying pipeline between the residual liquid conveying pump and the oil and gas recovery machine.
[0014] The second inlet at the top of the above-mentioned discharge buffer tank is fixedly connected to a second nitrogen pipeline. The lower outlet of the residual liquid tank is fixedly connected to the first material conveying pipeline between the residual liquid tank and the residual liquid conveying pump. The upper outlet of the residual liquid tank is fixedly connected to a second overflow pipeline. A second pressure gauge and a first level gauge are fixedly installed on the residual liquid tank.
[0015] The aforementioned discharge buffer tank is fixedly connected to the discharge pump and the fifth material conveying pipeline at the outlet of the fifth material conveying pipeline via a return pipeline. A third pressure gauge and a second level gauge are fixedly installed on the discharge buffer tank.
[0016] The above also includes a PLC controller, which is equipped with a DCS control system. The residual liquid transfer pump, discharge pump, first pressure gauge, first thermometer, second thermometer, second pressure gauge, first level gauge, third pressure gauge, and second level gauge are all electrically connected to the DCS control system.
[0017] This utility model has a reasonable and compact structure and is easy to use. It utilizes an oil and gas recovery machine with a stirrer to heat the bottom liquid of the distillation column under vacuum conditions to a temperature higher than that of the bottom liquid of existing distillation columns, thereby removing organic matter from the bottom liquid. Finally, the organic matter is further separated and recycled, and the organic matter recovery rate can reach more than 80%, thereby achieving the purpose of reducing waste generation and reusing waste. Attached Figure Description
[0018] Appendix Figure 1 This is a schematic diagram of the process flow of this utility model.
[0019] Appendix Figure 1 The codes in the diagram are as follows: 1 for residual liquid tank, 2 for oil and gas recovery machine, 3 for condenser, 4 for discharge buffer tank, 5 for first material conveying pipeline, 6 for second material conveying pipeline, 7 for third material conveying pipeline, 8 for fourth material conveying pipeline, 9 for fifth material conveying pipeline, 10 for residual liquid conveying pump, 11 for discharge pump, 12 for agitator, 13 for discharge pipeline, 14 for first nitrogen pipeline, 15 for first overflow pipeline, 16 for cooling water supply pipeline, 17 for cooling water return pipeline, 18 for first pressure gauge, 19 for first thermometer, 20 for second thermometer, 21 for drain pipeline, 22 for second overflow pipeline, 23 for second pressure gauge, 24 for first level gauge, 25 for negative pressure extraction pipeline, 26 for second nitrogen pipeline, 27 for return pipeline, 28 for third pressure gauge, and 29 for second level gauge. Detailed Implementation
[0020] This utility model is not limited to the following embodiments, and the specific implementation method can be determined according to the technical solution of this utility model and the actual situation.
[0021] Unless otherwise specified, all equipment and devices used in this invention are existing, publicly known, and commonly used equipment and devices in the field.
[0022] In this utility model, for ease of description, the description of the relative positions of the components is based on the appendix to the specification. Figure 1 The layout is described using a diagrammatic method, such as the positional relationships of front, back, top, bottom, left, and right, which are based on the instructions attached. Figure 1 The orientation of the layout is determined by the direction of the map.
[0023] The present invention will be further described below with reference to the embodiments and accompanying drawings:
[0024] Example 1: As shown in the attached document Figure 1 As shown, the distillation column bottom material oil and gas recovery device includes a residual liquid tank 1, an oil and gas recovery machine 2, a condenser 3, and a discharge buffer tank 4. The top inlet of the residual liquid tank 1 is fixedly connected to a first material conveying pipeline 5. The bottom outlet of the residual liquid tank 1 is fixedly connected to the top first inlet of the oil and gas recovery machine 2 via a second material conveying pipeline 6. The top outlet of the oil and gas recovery machine 2 is fixedly connected to the top inlet of the condenser 3 via a third material conveying pipeline 7. The bottom outlet of the condenser 3 is fixedly connected to the top first inlet of the discharge buffer tank 4 via a fourth material conveying pipeline 8. The lower outlet of the discharge buffer tank 4 is fixedly connected to a fifth material conveying pipeline 9.
[0025] In this invention, the residue from the first distillation in the production of dichlorobenzene is collected in a residue tank 1. After entering the oil and gas recovery machine 2, the oil and gas recovery machine 2 effectively separates the organic matter and solid matter (mainly ferric chloride) in the residue. The separated organic matter is condensed by a condenser 3 and then enters a discharge buffer tank 4. After further separation and purification, it is reused.
[0026] The above-mentioned distillation column bottom oil and gas recovery device can be further optimized and / or improved according to actual needs:
[0027] Example 2: Its difference from Example 1 is as follows: (See attached) Figure 1 As shown, a residual liquid conveying pump 10 and a discharge pump 11 are fixedly installed on the second material conveying pipeline 6 and the fifth material conveying pipeline 9, respectively.
[0028] Depending on the requirements, the residual liquid transfer pump 10 and the discharge pump 11 can be diaphragm pumps.
[0029] Example 3: Its difference from Examples 1 to 2 is as follows: (See attached) Figure 1 As shown, the top outlet of the discharge buffer tank 4 is fixedly connected to a negative pressure suction pipeline 25.
[0030] As required, at -80 kPa (gauge pressure), the boiling point of the light organic components in the bottom liquid of the distillation column is approximately 170°C. The oil and gas recovery unit 2 utilizes the different boiling points of the materials under different saturated vapor pressures to achieve effective separation. Before the separation operation, the oil and gas recovery unit 2 uses the negative pressure extraction pipeline 25 to evacuate the system pressure of the entire distillation column bottom material oil and gas recovery unit to -80 kPa.
[0031] Example 4: Its difference from Examples 1 to 3 is as follows: (See attached) Figure 1 As shown, an agitator 12 is fixedly installed inside the oil and gas recovery machine 2, and a jacket is fixedly installed outside the oil and gas recovery machine 2. A heating component is fixedly installed inside the jacket.
[0032] As needed, the heating component uses a heating rod, which is a resistance heating element. When the oil and gas recovery machine 2 separates and recovers organic matter in the bottom residue of the tower, the stirrer 12 stirs the mixture and the heating component heats it up, which accelerates the evaporation and discharge of organic matter inside the bottom residue of the tower.
[0033] Example 5: It differs from Examples 1 to 4 in that, as shown in the appendix... Figure 1 As shown, the bottom outlet of the oil and gas recovery machine 2 is fixedly connected to the discharge pipeline 13, the top second inlet of the oil and gas recovery machine 2 is fixedly connected to the first nitrogen pipeline 14, and the upper outlet of the oil and gas recovery machine 2 is fixedly connected to the first overflow pipeline 15.
[0034] As needed, the oil and gas recovery machine 2 adopts intermittent separation operation. When the solids after the separation of the residual liquid in the tower need to be discharged from the oil and gas recovery machine 2, nitrogen is introduced into the oil and gas recovery machine 2 through the first nitrogen pipeline 14 to press out the separated solids from the oil and gas recovery machine 2.
[0035] Example 6: Its difference from Examples 1 to 5 is as follows: (See attached) Figure 1 As shown, a cooling water supply line 16 is fixedly connected to the bottom inlet of the condenser 3, and a cooling water return line 17 is fixedly connected to the top outlet of the condenser 3.
[0036] Example 7: Its difference from Examples 1 to 6 is as follows: (See attached) Figure 1 As shown, a first pressure gauge 18 and a first thermometer 19 are fixedly installed on the oil and gas recovery machine 2, and a second thermometer 20 is fixedly installed on the second material conveying pipeline 6 between the residual liquid conveying pump 10 and the oil and gas recovery machine 2.
[0037] As needed, when the oil and gas recovery machine 2 performs the separation operation of the bottom residue of the tower, the operating temperature is usually controlled at 200℃.
[0038] Example 8: It differs from Examples 1 to 7 in that: as shown in the appendix Figure 1 As shown, a drain line 21 is fixedly connected between the lower outlet of the residual liquid tank 1 and the second material conveying pipeline 6 between the residual liquid tank 1 and the residual liquid conveying pump 10. A second overflow pipeline 22 is fixedly connected to the upper outlet of the residual liquid tank 1. A second pressure gauge 23 and a first liquid level gauge 24 are fixedly installed on the residual liquid tank 1.
[0039] When the residual liquid tank 1 needs to be emptied and cleaned as needed, all the residual liquid at the bottom of the tower bottom of the residual liquid tank 1 is sent to the oil and gas recovery machine through the drain line 21.
[0040] Example 9: It differs from Examples 1 to 8 in that: as shown in the appendix Figure 1 As shown, the second nitrogen pipeline 26 is fixedly connected to the second inlet at the top of the discharge buffer tank 4. The return pipeline 27 is fixedly connected between the discharge buffer tank 4 and the fifth material conveying pipeline 9 between the discharge pump 11 and the outlet of the fifth material conveying pipeline 9. The third pressure gauge 28 and the second liquid level gauge 29 are fixedly installed on the discharge buffer tank 4.
[0041] If the organic matter in the discharge buffer tank 4 needs to be sent out as needed, nitrogen is introduced into the discharge buffer tank 4 through the second nitrogen pipeline 26. When the pressure in the discharge buffer tank 4 reaches the normal pressure (one standard atmosphere) by the third pressure gauge 28, the discharge pump 11 is started, and the organic matter is sent out through the discharge pump 11.
[0042] When the oil and gas recovery machine 2 performs the tower bottom residual liquid separation operation, it compares the increase value of the liquid level of the second liquid level gauge 29 on the discharge buffer tank 4 with the decrease value of the liquid level of the first liquid level gauge 24 on the residual liquid tank 1 to determine the separation status of the tower bottom residual liquid in the oil and gas recovery machine 2. When the volumes of the two are equal, the separation operation of the oil and gas recovery machine 2 is completed.
[0043] Example 10: It differs from Examples 1 to 9 in that, as shown in the appendix... Figure 1 As shown, it also includes a PLC controller, in which a DCS control system is installed. The residual liquid transfer pump 10, the discharge pump 11, the first pressure gauge 18, the first thermometer 19, the second thermometer 20, the second pressure gauge 23, the first level gauge 24, the third pressure gauge 28, and the second level gauge 29 are all electrically connected to the DCS control system.
[0044] Depending on the needs, the pipelines and equipment of the distillation column bottom material oil and gas recovery unit may also be equipped with conventional valves, thermometers, and pressure gauges known in the art, according to production requirements. The PLC controller can be a Siemens S7-1500, which is equipped with a Yokogawa CS3000 DCS control system.
[0045] The above technical features constitute various embodiments of this utility model, which have strong adaptability and implementation effect. Unnecessary technical features can be added or removed according to actual needs to meet the needs of different situations.
[0046] The usage process of this utility model embodiment is as follows: First, the residual liquid in the tower bottom enters the oil and gas recovery machine 2 through the residual liquid transfer pump 10 for gas-solid phase separation to obtain gaseous organic matter and ferric chloride solid; then, the gaseous organic matter enters the condenser 3, is condensed and stored in the discharge buffer tank 4, and the ferric chloride solid is sent out for packaging through the discharge pipeline 13; finally, the organic matter is sent out through the discharge pump 11.
Claims
1. A distillation column bottom oil and gas recovery device, characterized in that... It includes a residual liquid tank, an oil and gas recovery machine, a condenser, and a discharge buffer tank. The top inlet of the residual liquid tank is fixedly connected to a first material conveying pipeline. The bottom outlet of the residual liquid tank is fixedly connected to the first inlet of the top of the oil and gas recovery machine, the top outlet of the oil and gas recovery machine is fixedly connected to a third material conveying pipeline, the bottom outlet of the condenser is fixedly connected to the first inlet of the top of the discharge buffer tank, and the lower outlet of the discharge buffer tank is fixedly connected to a fifth material conveying pipeline.
2. The distillation column bottom material oil and gas recovery device according to claim 1, characterized in that... The second and fifth material conveying pipelines are respectively equipped with residual liquid conveying pumps and discharge pumps.
3. The distillation column bottom material oil and gas recovery device according to claim 1 or 2, characterized in that... The top outlet of the discharge buffer tank is fixedly connected to a negative pressure extraction pipeline.
4. The distillation column bottom material oil and gas recovery device according to claim 3, characterized in that... An agitator is fixedly installed inside the oil and gas recovery machine, and a jacket is fixedly installed outside the oil and gas recovery machine. A heating component is fixedly installed inside the jacket.
5. The distillation column bottom material oil and gas recovery device according to claim 1, 2, or 4, characterized in that... The bottom outlet of the oil and gas recovery machine is fixedly connected to a discharge pipeline, the second inlet at the top of the oil and gas recovery machine is fixedly connected to a first nitrogen pipeline, and the upper outlet of the oil and gas recovery machine is fixedly connected to a first overflow pipeline.
6. The distillation column bottom material oil and gas recovery device according to claim 5, characterized in that... The bottom inlet of the condenser is fixedly connected to a cooling water supply line, and the top outlet of the condenser is fixedly connected to a cooling water return line.
7. The distillation column bottom material oil and gas recovery device according to claim 2, 4, or 6, characterized in that... The oil and gas recovery machine is equipped with a first pressure gauge and a first thermometer, and a second thermometer is fixedly installed on the second material conveying pipeline between the residual liquid conveying pump and the oil and gas recovery machine.
8. The distillation column bottom material oil and gas recovery device according to claim 7, characterized in that... A drain line is fixedly connected between the lower outlet of the residual liquid tank and the first material conveying pipeline between the residual liquid tank and the residual liquid conveying pump. A second overflow line is fixedly connected to the upper outlet of the residual liquid tank. A second pressure gauge and a first level gauge are fixedly installed on the residual liquid tank.
9. The distillation column bottom material oil and gas recovery device according to claim 2, 4, 6, or 8, characterized in that... The second inlet at the top of the discharge buffer tank is fixedly connected to the second nitrogen pipeline. The discharge buffer tank is fixedly connected to the fifth material conveying pipeline between the discharge pump and the outlet of the fifth material conveying pipeline. The discharge buffer tank is fixedly equipped with a third pressure gauge and a second level gauge.
10. The distillation column bottom material oil and gas recovery device according to claim 9, characterized in that... It also includes a PLC controller, which is equipped with a DCS control system. The residual liquid transfer pump, discharge pump, first pressure gauge, first thermometer, second thermometer, second pressure gauge, first level gauge, third pressure gauge, and second level gauge are all electrically connected to the DCS control system.