CN214088348U - Device for recovering phenol in tar through multi-effect rectification - Google Patents
Device for recovering phenol in tar through multi-effect rectification Download PDFInfo
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- CN214088348U CN214088348U CN202022464282.4U CN202022464282U CN214088348U CN 214088348 U CN214088348 U CN 214088348U CN 202022464282 U CN202022464282 U CN 202022464282U CN 214088348 U CN214088348 U CN 214088348U
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Abstract
The utility model relates to a device of phenol in multiple-effect rectification recovery tar, including 1# recovery tower, 2# recovery tower, condenser, flow control valve, liquid level control valve, gas-liquid separation subcooler, 1# recovery tower reboiler, low temperature condenser, 2# recovery tower reboiler, 2# recovery tower condenser, 1# recovery tower vacuum system and 2# recovery tower vacuum system. In the phenol recovery method, a 1# recovery tower and a 2# recovery tower are operated under negative pressure, part of steam at the top of the 1# recovery tower passes through a flow control valve and goes to a reboiler of the 2# recovery tower, part of steam is condensed by a condenser, two condensate flows to a gas-liquid separation subcooler, the liquid phase part returns to the 1# recovery tower, and the part of steam is used as the feed of the 2# recovery tower. The utility model discloses economic benefits and social benefits rectification compares with traditional phenol rectification recovery method, reduces the total energy consumption of whole rectifying column system among the phenol recovery process by a wide margin, saves operating cost, reaches energy-conserving increase purpose.
Description
Technical Field
The utility model belongs to the green energy-saving technology, in particular to a device for recovering phenol in tar by multi-effect rectification.
Background
Rectification is an industrial separation method with the widest application, and is widely applied to industrial departments such as chemical industry, petroleum, food, light industry and the like, and although the development of science and technology and the industrial application of a novel separation technology begin, the domination position of the rectification technology cannot be passively shaken within a certain period. The rectification separation technology is mature and easy to industrialize, but has the defect of high energy consumption. In the traditional rectification separation, the input energy consumption accounts for more than 40% of the total industrial energy consumption, which is not negligible in the 21 st century with increasingly short energy sources.
The phenol tar is a byproduct of a device for preparing phenol acetone by using cumene as a raw material, and is a distillation residue after phenol and acetone are separated as a reaction product. The phenol is separated from the phenol-containing tar, and is often used for rectification, so that the energy consumption is large, and the energy consumption of public works is also large.
Patent CN101835732 discloses a process for recovering acetophenone during the production of phenol, which comprises treating one or more alkylbenzenes comprising sec-butylbenzene to produce a feed comprising phenol and acetophenone, separating a crude material fraction from the feed under crude phenol separation conditions effective to produce a crude phenol heavies and separating acetophenone directly from the crude material fraction under azeotropic distillation conditions. The patent is contrastively analyzed, phenol and acetophenone are obtained by rectifying and purifying a system for producing phenol and acetophenone by sec-butylbenzene or various alkylbenzenes, and the related system is not a system taking cumene as a raw material, so that the purified raw material has different compositions and different purification procedures and requirements. And the purification adopts a conventional rectification scheme, and does not relate to rectification energy integration.
Patent CN102153092B discloses a trichlorosilane purification device and process integrating heat pump rectification and multiple-effect rectification, wherein tower top steam of a high-pressure tower, namely a heavy-component removal tower, is used for heating tower kettle liquid of a low-pressure tower, namely a light-component removal tower, the tower top steam of the heavy-component removal tower is condensed, the process is multiple-effect rectification, meanwhile, the tower top steam of the light-component removal tower is heated and boosted by a compressor and then is used for heating the tower kettle liquid of the heavy-component removal tower, the tower top steam of the light-component removal tower is condensed, and the process is a heat pump rectification process. Compared with the patent, the process realizes the integration of heat pump rectification and multi-effect rectification by adding one compressor. The compressor cannot adjust the negative pressure operation condition of the tower, so the rectification device and the process can only operate under normal pressure or pressurization condition, and are not suitable for multi-effect rectification operation under reduced pressure.
SUMMERY OF THE UTILITY MODEL
The utility model aims at solving the problems and providing a device for recovering phenol in tar by multi-effect rectification so as to reduce the energy consumption of recovering phenol in tar.
The purpose of the utility model is realized through the following technical scheme:
a device for recovering phenol in tar by multi-effect rectification comprises a 1# recovery tower and a 2# recovery tower, and further comprises a 1# recovery tower condenser, a gas-liquid separation subcooler, a low-temperature condenser, a 1# recovery tower vacuum system, a 2# recovery tower reboiler, a 2# recovery tower condenser and a 2# recovery tower vacuum system;
the 2# recovery tower reboiler is arranged at the bottom of the 2# recovery tower, one part of the gas phase material at the top of the 1# recovery tower directly enters the 2# recovery tower reboiler through a pipeline for heat exchange, and the other part of the gas phase material enters the 1# recovery tower condenser;
the 2# recovery tower reboiler and the steam condensate of the 1# recovery tower condenser jointly enter the gas-liquid separation subcooler through a pipeline;
the upper gas-phase material of the gas-liquid separation subcooler is sequentially connected with the low-temperature condenser and the No. 1 recovery tower vacuum system through pipelines, part of the lower liquid-phase material of the gas-liquid separation subcooler reflows to the top of the No. 1 recovery tower, and part of the lower liquid-phase material enters the No. 2 recovery tower;
2# recovery tower top gas phase material passes through the pipeline and connects gradually 2# recovery tower condenser and 2# recovery tower vacuum system, the top of the tower gas phase material process after 2# recovery tower condenser condenses, partly backward flow to 2# recovery tower, and partly is extracted and is collected.
Further, the bottom of the No. 1 recovery tower is provided with a No. 1 recovery tower reboiler.
Furthermore, a flow regulating valve is arranged in a pipeline connecting the gas-phase material at the top of the No. 1 recovery tower and the reboiler of the No. 2 recovery tower.
Further, a part of liquid phase materials at the lower part of the gas-liquid separation subcooler are pumped into the top of the No. 1 recovery tower through a reflux pump, and a part of the liquid phase materials are pumped into the No. 2 recovery tower as feeding materials.
Furthermore, a liquid level regulating valve is arranged in a pipeline for the liquid-phase material of the gas-liquid separation subcooler to enter the No. 2 recovery tower.
Further, the No. 1 recovery tower and the No. 2 recovery tower are both under negative pressure and are respectively regulated by the No. 1 recovery tower vacuum system and the No. 2 recovery tower vacuum system.
The method for recovering phenol in tar by multi-effect rectification is carried out by adopting the device, and specifically comprises the following steps:
the method comprises the following steps that a tar raw material containing phenol enters a No. 1 recovery tower, the operation pressure of the No. 1 recovery tower is controlled to be negative pressure operation through a No. 1 recovery tower vacuum system, the material is heated and vaporized in the No. 1 recovery tower, a part of gas-phase material at the top of the No. 1 recovery tower enters a No. 2 recovery tower reboiler for heat exchange and serves as an energy source of the No. 2 recovery tower kettle reboiler, and a part of gas-phase material enters a No. 1 recovery tower condenser;
the reboiler of the No. 2 recovery tower and the steam condensate of the condenser of the No. 1 recovery tower enter a gas-liquid separation subcooler together, and gas-phase materials in the gas-liquid separation subcooler enter a vacuum system of the No. 1 recovery tower through a low-temperature condenser; a part of liquid phase materials in the gas-liquid separation subcooler flow back to the top of the No. 1 recovery tower, a part of liquid phase materials enter the No. 2 recovery tower as a feed, and tower kettle materials of the No. 1 recovery tower are extracted to the outside and collected;
the operating pressure of the No. 2 recovery tower is controlled to be negative pressure operation through a No. 2 recovery tower vacuum system, liquid phase materials entering the No. 2 recovery tower are heated and vaporized, gas phase materials at the top of the tower are condensed through a No. 2 recovery tower condenser, one part of condensate flows back to the No. 2 recovery tower, one part of condensate is extracted and collected to obtain high-purity phenol recovery liquid, and heavy components in a tower kettle of the No. 2 recovery tower are extracted and collected outside the tower.
Further, the operating pressure of the No. 1 recovery tower is 5-90kPa absolute, and the preferred operating pressure is 40-60kPa absolute.
Further, the operating pressure of the No. 2 recovery tower is 1-70kPa in absolute pressure, and the preferred operating pressure is 20-40 kPa.
Further, the mass content of phenol in the phenol recovery liquid is more than 99%.
The utility model discloses double-effect rectification utilizes the latent heat of high-pressure tower top steam to provide the heat integration rectification system of heat for the reboiler of low-pressure column. Compared with the conventional rectification, the method greatly improves the utilization rate of energy, saves the energy consumption of a rectification device to a greater extent, and has high quality and high yield of the rectified product.
The utility model discloses a key lies in, the relation of connection between 1# recovery tower and the 2# recovery tower, through the utility model discloses device and technology, 1# recovery tower top of the tower gas phase material directly gets into 2# recovery tower reboiler through pipeline partly and carries out the heat transfer, another part gets into 1# recovery tower condenser, 2# recovery tower reboiler and 1# recovery tower condenser's steam condensate passes through the pipeline and gets into the gas-liquid separation subcooler jointly, gas-liquid separation subcooler lower part liquid phase material partly flows back to 1# recovery tower top of the tower, partly gets into 2# recovery tower, regard 1# recovery tower top of the tower steam as the energy source of 2# recovery tower kettle reboiler, show and reduce 1# recovery tower top of the tower refrigerant volume and cancel 2# recovery tower kettle reboiler heat medium volume, reduce rectification system working costs. And the gas-liquid separation subcooler is used as a collecting tank of the condensate of the tower top steam of the No. 1 recovery tower so as to maintain the pressure of the No. 1 recovery tower under the negative pressure operation condition to be stable, and the steam quantity of the tower top steam of the No. 1 recovery tower to the No. 2 recovery tower reboiler 10 can be adjusted.
Compared with the prior art, the utility model discloses there is following advantage:
(1) compared with the scheme of cracking and purifying phenol by phenol tar, the utility model adopts the negative pressure rectification method, avoids cracking heavy components, can separate phenol by two towers, and has simple process flow;
(2) compared with the scheme of purifying phenol by rectification, the utility model discloses a multiple-effect rectification method effectively reduces the total energy consumption of rectification system, reduces the operating cost.
Drawings
FIG. 1 is a schematic flow chart of the device for recovering phenol from tar by multi-effect rectification according to the present invention;
in the figure: 1# recovery column 1; 2# recovery column 2; 1# recovery column condenser 3; a flow regulating valve 4; a liquid level regulating valve 5; a gas-liquid separation subcooler 6; a reflux pump 7; 1# recovery column reboiler 8; a low-temperature condenser 9; 2# recovery column reboiler 10; 2# recovery column condenser 11; 1# recovery column vacuum system 12; recovery column vacuum system # 2 13.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings and specific embodiments. It should not be understood that the scope of the above-described subject matter of the present invention is limited to the examples. Various substitutions and alterations can be made without departing from the technical spirit of the invention, and all changes and modifications can be made by the ordinary technical knowledge and the conventional means in the field.
Referring to fig. 1, a device for recovering phenol in tar by multi-effect rectification, which comprises a # 1 recovery tower 1 and a # 2 recovery tower 2, and further comprises a # 1 recovery tower condenser 3, a gas-liquid separation subcooler 6, a low-temperature condenser 9, a # 1 recovery tower vacuum system 12, a # 2 recovery tower reboiler 10, a # 2 recovery tower condenser 11 and a # 2 recovery tower vacuum system 13; the bottom of the No. 1 recovery tower is provided with a No. 1 recovery tower reboiler 8.
The connection relationship among the components is as follows: the 2# recovery tower reboiler 10 is arranged at the bottom of the 2# recovery tower 2, part of the gas phase material at the top of the 1# recovery tower 1 directly enters the 2# recovery tower reboiler 10 for heat exchange through a pipeline, and the other part of the gas phase material enters the 1# recovery tower condenser 3; a flow regulating valve 4 is arranged in a pipeline connecting the gas phase material at the top of the 1# recovery tower 1 and a 2# recovery tower reboiler 10, and the steam condensate of the 2# recovery tower reboiler 10 and a 1# recovery tower condenser 3 jointly enters a gas-liquid separation subcooler 6 through the pipeline; the upper gas phase material of the gas-liquid separation subcooler 6 is sequentially connected with the low-temperature condenser 9 and the No. 1 recovery tower vacuum system 12 through pipelines, part of the lower liquid phase material of the gas-liquid separation subcooler 6 is pumped into the top of the No. 1 recovery tower 1 through the reflux pump 7, part of the lower liquid phase material is pumped into the No. 2 recovery tower 2 as a feed material, and the liquid phase material of the gas-liquid separation subcooler 6 is provided with a liquid level regulating valve 5 in the pipeline for entering the No. 2 recovery tower 2. 2# recovery tower 2 top gas phase material passes through the pipeline and connects gradually 2# recovery tower condenser 11 and 2# recovery tower vacuum system 13, and the top gas phase material is through 2# recovery tower condenser 11 condensation back, and partly backward flow is to 2# recovery tower 2, and partly is extracted and is collected.
The method for recovering phenol in tar by adopting the device specifically comprises the following steps:
feeding a tar raw material containing phenol into a No. 1 recovery tower 1, controlling the operation pressure of the No. 1 recovery tower 1 to be negative pressure operation through a No. 1 recovery tower vacuum system 12, controlling the operation pressure of the No. 1 recovery tower 1 to be 5-90kPa, preferably controlling the operation pressure to be 40-60kPa, heating and vaporizing the material in the No. 1 recovery tower 1, feeding a part of gas phase material at the top of the No. 1 recovery tower 1 into a No. 2 recovery tower reboiler 10 for heat exchange and serving as an energy source of a No. 2 recovery tower kettle reboiler 10, and feeding a part of gas phase material into a No. 1 recovery tower condenser 3;
the 2# recovery tower reboiler 10 and the steam condensate of the 1# recovery tower condenser 3 enter the gas-liquid separation subcooler 6 together, and gas-phase materials in the gas-liquid separation subcooler 6 enter the 1# recovery tower vacuum system 12 through the low-temperature condenser 9; a part of liquid phase materials in the gas-liquid separation subcooler 6 flow back to the top of the No. 1 recovery tower 1, a part of liquid phase materials enter the No. 2 recovery tower 2 as a feed, and materials in the bottom of the No. 1 recovery tower 1 are extracted to the outside and collected;
the operating pressure of a No. 2 recovery tower 2 is controlled to be negative pressure operation through a No. 2 recovery tower vacuum system 13, the operating pressure of the No. 2 recovery tower 2 is absolute pressure 1-70kPa, the preferred operating pressure is 20-40kPa, liquid phase materials entering the No. 2 recovery tower 2 are heated and vaporized, gas phase materials at the top of the tower are condensed through a No. 2 recovery tower condenser 11, one part of condensate flows back to the No. 2 recovery tower 2, one part of condensate is collected by extraction, high-purity phenol recovery liquid with the phenol mass content of more than 99% in the phenol recovery liquid is obtained, and heavy components at the bottom of the No. 2 recovery tower 2 are collected outside the tower.
The following are specific application examples
Example 1
The device and the process are adopted as shown in figure 1. The tar raw material containing phenol comprises the following components: 19.9 percent of phenol, 10.3 percent of acetophenone, 0.1 percent of dimethylphenol, 21.7 percent of cumylphenol and 48.0 percent of other heavy components (all in mass proportion). The raw material enters a No. 1 recovery tower for separation and recovery. The reboiler of the 1# recovery tower adopts high-pressure steam, the material is heated and vaporized through the reboiler 8 of the 1# recovery tower, a part of the steam at the top of the tower passes through a flow regulating valve 4 and enters the reboiler 10 of the 2# recovery tower, the steam condensate thereof enters a gas-liquid separation subcooler 6, the rest steam passes through a condenser 3 of the 1# recovery tower and a liquid level regulating valve 5 and enters the gas-liquid separation subcooler 6, and the gas-phase material in the gas-liquid separation subcooler 6 enters a vacuum system 12 of the 1# recovery tower through a low-temperature condenser 9; and a part of the liquid-phase material in the gas-liquid separation subcooler 6 is pumped into the top of the No. 1 recovery tower through a reflux pump 7, and a part of the liquid-phase material is pumped into the No. 2 recovery tower as a feed. And (4) extracting materials at the tower bottom of the 1# recovery tower to the outside and collecting the materials.
The liquid phase material of the gas-liquid separation subcooler 6 enters a No. 2 recovery tower. The tower operating pressure is controlled by a 2# recovery tower vacuum system 13, materials are heated and vaporized by a 2# recovery tower reboiler 10, steam at the top of the tower is condensed by a 2# recovery tower condenser 11, part of condensate flows back, and part of condensate is extracted and collected to obtain phenol recovery liquid with higher purity, wherein the purity of phenol can reach 99.1%. And (4) extracting heavy components in the tower kettle of the 2# recovery tower to the outside and collecting the heavy components.
Compared with the conventional double-tower rectification energy consumption, the method has the specific energy consumption shown in table 1.
Table 1 comparison of example 1 with conventional distillation energy consumption
| Item | Unit of | Conventional double column rectification | EXAMPLE 1 double effect rectification |
| Steam generating device | t/h | 3.5 | 2.3 |
| Circulating water | t/h | 109 | 40 |
| Total energy saving rate | ％ | / | 36％ |
As can be seen from Table 1, in the double-effect rectification adopted in the embodiment, the overhead steam of the recovery tower 1 serves as the heat source of the reboiler at the tower bottom of the recovery tower 2, and compared with the conventional double-tower rectification, the comprehensive energy consumption is reduced by 36%.
Example 2
According to the conditions and steps of the embodiment 1, only the raw material composition is changed, the composition of the raw material is 23.0 percent of phenol, 11.3 percent of acetophenone, 0.1 percent of dimethylphenol, 22.3 percent of cumylphenol and 43.3 percent of other heavy components, the phenol recovery liquid with higher purity is obtained, and the purity of the phenol is up to 99 percent.
The energy consumption of the double-effect rectification is compared with that of the conventional rectification in the following table.
The specific energy consumption of this example compared to the conventional double column distillation energy consumption is shown in Table 2.
Table 2 comparison of example 2 with conventional distillation energy consumption
| Item | Unit of | Conventional double column rectification | EXAMPLE 2 double effect rectification |
| Steam generating device | t/h | 4.2 | 2.7 |
| Circulating water | t/h | 120 | 46 |
| Total energy saving rate | ％ | / | 37％ |
As can be seen from the above table, in the double-effect rectification adopted in this embodiment, the steam at the top of the recovery tower is used as the heat source of the reboiler at the bottom of the recovery tower, and compared with the conventional double-tower rectification, the comprehensive energy consumption is reduced by 37%.
The embodiments described above are intended to facilitate the understanding and use of the invention by those skilled in the art. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above embodiments, and those skilled in the art should make improvements and modifications within the scope of the present invention according to the disclosure of the present invention.
Claims (6)
1. A device for recovering phenol in tar by multi-effect rectification is characterized by comprising a 1# recovery tower (1) and a 2# recovery tower (2), and further comprising a 1# recovery tower condenser (3), a gas-liquid separation subcooler (6), a low-temperature condenser (9), a 1# recovery tower vacuum system (12), a 2# recovery tower reboiler (10), a 2# recovery tower condenser (11) and a 2# recovery tower vacuum system (13);
the 2# recovery tower reboiler (10) is arranged at the bottom of the 2# recovery tower (2), one part of the gas phase material at the top of the 1# recovery tower (1) directly enters the 2# recovery tower reboiler (10) for heat exchange through a pipeline, and the other part of the gas phase material enters the 1# recovery tower condenser (3);
the 2# recovery tower reboiler (10) and the steam condensate of the 1# recovery tower condenser (3) jointly enter the gas-liquid separation subcooler (6) through a pipeline;
the upper gas-phase material of the gas-liquid separation subcooler (6) is sequentially connected with the low-temperature condenser (9) and the No. 1 recovery tower vacuum system (12) through pipelines, one part of the lower liquid-phase material of the gas-liquid separation subcooler (6) reflows to the top of the No. 1 recovery tower (1), and the other part of the lower liquid-phase material enters the No. 2 recovery tower (2);
2# recovery tower (2) top of the tower gas material passes through the pipeline and connects gradually 2# recovery tower condenser (11) and 2# recovery tower vacuum system (13), top of the tower gas material pass through after 2# recovery tower condenser (11) condensation, partly flow back to 2# recovery tower (2), and partly are adopted and are collected.
2. The device for recovering phenol in tar by multi-effect rectification as claimed in claim 1, wherein a 1# recovery tower reboiler (8) is arranged at the bottom of the 1# recovery tower.
3. The device for recovering phenol in tar by multi-effect rectification according to claim 1, characterized in that a flow control valve (4) is arranged in a pipeline connecting the gas phase material at the top of the No. 1 recovery tower (1) and the 2 No. recovery tower reboiler (10).
4. The device for recovering phenol in tar by multi-effect rectification according to claim 1, characterized in that part of the liquid phase material at the lower part of the gas-liquid separation subcooler (6) is pumped into the top of the No. 1 recovery tower (1) through a reflux pump (7), and part of the liquid phase material is pumped into the No. 2 recovery tower (2) as a feed.
5. The device for recovering phenol in tar by multi-effect rectification according to claim 4, characterized in that a liquid level regulating valve (5) is arranged in a pipeline for liquid phase materials of the gas-liquid separation subcooler (6) to enter the No. 2 recovery tower (2).
6. The device for recovering phenol in tar by multi-effect rectification as claimed in claim 1, wherein the 1# recovery tower (1) and the 2# recovery tower (2) are both under negative pressure and are respectively regulated by the 1# recovery tower vacuum system (12) and the 2# recovery tower vacuum system (13).
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| CN202022464282.4U CN214088348U (en) | 2020-10-30 | 2020-10-30 | Device for recovering phenol in tar through multi-effect rectification |
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| CN202022464282.4U CN214088348U (en) | 2020-10-30 | 2020-10-30 | Device for recovering phenol in tar through multi-effect rectification |
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