CN110759804B - Device and method for extracting, rectifying and concentrating dimethylnaphthalene through lower side line - Google Patents
Device and method for extracting, rectifying and concentrating dimethylnaphthalene through lower side line Download PDFInfo
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- CN110759804B CN110759804B CN201910954305.9A CN201910954305A CN110759804B CN 110759804 B CN110759804 B CN 110759804B CN 201910954305 A CN201910954305 A CN 201910954305A CN 110759804 B CN110759804 B CN 110759804B
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- C07C7/04—Purification; Separation; Use of additives by distillation
- C07C7/05—Purification; Separation; Use of additives by distillation with the aid of auxiliary compounds
- C07C7/08—Purification; Separation; Use of additives by distillation with the aid of auxiliary compounds by extractive distillation
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Abstract
The invention discloses a device for extracting, rectifying and concentrating dimethylnaphthalene on a lower side line, which comprises a rectifying tower and a recovery tower communicated with the rectifying tower; the rectifying tower comprises a first inlet for raw materials to enter, a second inlet for an extracting agent to enter, a first outlet arranged at the bottom end of the rectifying tower, a second outlet arranged at the top end of the rectifying tower and a third outlet arranged at the side edge of the rectifying tower; the recovery tower is provided with a third inlet communicated with the second outlet, a fourth outlet arranged at the top end of the recovery tower and communicated with the second inlet, and a fifth outlet arranged at the bottom end of the recovery tower. The device has simple structure, and the device can effectively save investment cost and reduce energy consumption by concentrating dimethylnaphthalene in the catalytic cracking light cycle oil LCO.
Description
Technical Field
The invention relates to a chemical extractive distillation separation device and a separation method, in particular to a device and a method for concentrating dimethylnaphthalene by lower side line extractive distillation.
Background
The annual processing capacity of a Chinese catalytic cracking (FCC) unit exceeds 1 hundred million tons, and the annual yield of Light Cycle Oil (LCO) exceeds 1000 million tons. The light cycle oil is used as the oil for recycling in the oil refining process as the name implies, and is not generally externally arranged. The catalytic cracking Light Cycle Oil (LCO) is different along with different cracking raw materials, cracking depth and cracking process, has extremely complex composition, wide distillation range, dark color and large peculiar smell. Currently, catalytic cracking Light Cycle Oil (LCO) mainly has the following applications: the diesel oil is used as diesel blend oil or directly used as fuel oil; the LCO Unicracking process of UOP company adopts a hydrocracking process with one-way one-time pass and partial conversion to produce ultra-low sulfur gasoline (ULSG) and ultra-low sulfur diesel (ULSD); the FD2G technology developed by China petrochemical and petrochemical research institute takes LCO as raw material to produce high octane number (RON >90) gasoline fraction and ultralow sulfur high-quality diesel oil with the sulfur mass fraction of less than 10 mu g/g and the cetane number of 10-30 units higher than that of crude oil; the RLG technology can adopt process flows of one-time pass, integrated two-stage method, partial fraction circulation and the like according to the property of raw oil and the target requirement of products, the technology comprises a scheme for producing gasoline to the maximum extent and a scheme for producing dimethylbenzene (BTX), and can also produce low-sulfur clean diesel blending components; the LCO-X process is primarily designed to convert naphtha range of materials to xylenes and benzene by cracking, while simultaneously cracking unconverted non-aromatics to liquefied petroleum gas, leaving unconverted LCO mass fraction less than 5%, and separating the materials from hydrotreating conversion and aromatics maximization by stripping and fractionation columns. Therefore, the comprehensive utilization of the catalytic cracking Light Cycle Oil (LCO) becomes the key point of deep processing of petrochemical enterprises, great economic benefit and environmental benefit are generated, and the improvement and development of the catalytic cracking (FCC) diesel oil production process are deeply influenced.
The traditional production process mainly processes circulating oil (LCO) through catalytic cracking and disproportionation to convert heavy aromatics into gasoline, diesel oil or BTX, wastes high value-added naphthalene compounds in the LCO, particularly methylnaphthalene and dimethylnaphthalene, wherein dimethylnaphthalene has a plurality of isomers, the boiling point range is 262-270 ℃, the boiling point of 2-ethylnaphthalene is 258 ℃, and the 2-ethylnaphthalene is difficult to remove by common rectification due to small boiling point difference. The methods for extracting and concentrating dimethylnaphthalene reported at present comprise a cryogenic crystallization method, an extraction/alkylation method, a cyclodehydrogenation method and a combined extraction and rectification method. The method has the problems of complex process or low purity and yield and the like.
Disclosure of Invention
The invention aims to: the invention aims to provide a device and a method which can effectively concentrate dimethylnaphthalene in LCO bicyclic aromatic hydrocarbon and have higher content and yield of the concentrated dimethylnaphthalene.
The technical scheme is as follows: the invention relates to a device for extracting, rectifying and concentrating dimethylnaphthalene on a lower side line, which comprises a rectifying tower and a recovery tower communicated with the rectifying tower;
the rectifying tower comprises a first inlet for raw materials to enter, a second inlet for an extracting agent to enter, a first outlet arranged at the bottom end of the rectifying tower, a second outlet arranged at the top end of the rectifying tower and a third outlet arranged at the side edge of the rectifying tower;
The recovery tower is provided with a third inlet communicated with the second outlet, a fourth outlet arranged at the top end of the recovery tower and communicated with the second inlet, and a fifth outlet arranged at the bottom end of the recovery tower.
The third exit of rectifying column is provided with the collecting vat, distribute a plurality of steam guide pipe and overflow pipe in the collecting vat, air duct and overflow pipe alternately evenly distributed, the side line discharge gate is connected to the collecting vat bottom.
The method for extracting, rectifying and concentrating the dimethylnaphthalene by using the device comprises the following steps:
(a) the raw materials enter the rectifying tower from a first inlet of the rectifying tower (1), the extracting agent is introduced from a second inlet, the pressure at the bottom of the tower top of the rectifying tower is controlled to be 0.005MPa, the pressure at the bottom of the tower bottom of the rectifying tower is controlled to be 0.010MPa, and the reflux ratio is 3-5: 1;
(b) and (3) introducing an extracting agent from a third inlet of the recovery tower, controlling the pressure at the top of the recovery tower to be 0.1-0.105 MPa, the pressure at the bottom of the recovery tower (2) to be 0.105-0.115 MPa, the temperature at the top of the recovery tower to be 80.1-82.5 ℃, and the temperature at the bottom of the recovery tower to be 253.2-255.6 ℃.
In the step (a), the top temperature of the rectifying tower (1) is 93.4-95.8 ℃, the side temperature of the rectifying tower is 161.2-163.5 ℃, and the bottom temperature of the rectifying tower is 176.3-178.7 ℃.
In the step (a), the plate extraction of the rectifying tower is 90-110 blocks.
In step (a), the extractant is acetonitrile.
The first inlet is higher than the second inlet.
The height of the third outlet is lower than the height of the second inlet.
Has the advantages that: (1) the device has simple structure, and the device can effectively save investment cost and reduce energy consumption by concentrating dimethylnaphthalene in catalytic cracking Light Cycle Oil (LCO); (2) the invention extracts and concentrates the dimethylnaphthalene by side-line extraction and rectification, thereby achieving the purposes of simplifying the separation process and simultaneously improving the purity and the yield of the dimethylnaphthalene.
Drawings
FIG. 1 is a schematic structural diagram of a lower side line extractive distillation dimethylnaphthalene concentration device in the invention;
FIG. 2 is a schematic view of the structure of the collecting tank of the present invention.
Detailed Description
Example 1: as shown in figure 1, the device for extracting, rectifying and concentrating dimethylnaphthalene on the lower side line comprises a rectifying tower 1 and a recovery tower 2 communicated with the rectifying tower 1;
the rectifying tower 1 comprises a first inlet 101 for raw materials to enter, a second inlet 102 for an extractant to enter, a first outlet 103 arranged at the bottom end of the rectifying tower 1, a second outlet 104 arranged at the top end of the rectifying tower 1 and a third outlet 105 arranged at the side edge of the rectifying tower 1, wherein the first inlet 101 is higher than the height of the second inlet 102, the third outlet 105 is positioned at the middle lower part of the rectifying tower 1, the height of the third outlet 105 is lower than that of the second inlet 102, a collecting tank 3 is arranged at the third outlet 105 of the rectifying tower 1, as shown in fig. 2, a plurality of steam guide pipes 301 and overflow pipes 302 are distributed in the collecting tank 3, the gas guide pipes 301 and the overflow pipes 302 are uniformly distributed in a crossed manner, and the bottom of the collecting tank 3 is connected with a side line discharge port 303.
The recovery tower 2 is provided with a third inlet 201 communicated with the second outlet 104, a fourth outlet 202 arranged at the top end of the recovery tower 2 and communicated with the second inlet 102, and a fifth outlet 203 arranged at the bottom end of the recovery tower 2.
The method for concentrating dimethyl by extractive distillation by using the device in the embodiment 1 comprises the following steps:
(a) raw materials enter a rectifying tower 1 from a first inlet 101 of the rectifying tower 1, an extracting agent is introduced from a second inlet 102, the pressure of the bottom of the tower top of the rectifying tower 1 is controlled to be 0.005MPa, the pressure of the bottom of the rectifying tower 1 is controlled to be 0.010MPa, the plate extraction rate of the rectifying tower 1 is 90-110, and the reflux ratio is 3-5: 1, the top temperature of a rectifying tower 1 is 93.4-95.8 ℃, the side temperature of the rectifying tower 1 is 161.2-163.5 ℃, and the bottom temperature of the rectifying tower 1 is 176.3-178.7 ℃;
(b) and (2) feeding an extractant acetonitrile from a third inlet 201 of the recovery tower 2, controlling the pressure at the top of the recovery tower 2 to be 0.1-0.105 MPa, the pressure at the bottom of the recovery tower 2 to be 0.105-0.115 MPa, the temperature at the top of the recovery tower 2 to be 80.1-82.5 ℃, the temperature at the bottom of the recovery tower 2 to be 253.2-255.6 ℃, and feeding the extractant acetonitrile into the rectifying tower 1 from a fourth outlet 202 after the extractant acetonitrile is recovered by the recovery tower 2.
Application example 1: the residual fraction with the mass content of the dimethylnaphthalene of 62.45%, the mass content of the 2-ethylnaphthalene of 16.85% and the mass content of the trimethylnaphthalene of 5.99% is taken as a raw material and enters the rectifying tower 1 from a first inlet 101 positioned at the middle upper part of the rectifying tower 1.
The first outlet 103 at the top end of the rectifying tower 1 is a discharge hole for 2-ethylnaphthalene and light components above the ethylnaphthalene, the second inlet 102 arranged in the middle of the rectifying tower 1 is used as a feed inlet for extracting agent acetonitrile, the third outlet 105 arranged at the middle lower part of the rectifying tower 1 is used as a side line discharge section, the first outlet 103 used for sending out heavy components below trimethylnaphthalene is arranged at the bottom end of the rectifying tower 1, and the bottom of the collecting tank 3 is connected with the side line third outlet 105.
The top end of the recovery tower is provided with a fourth outlet 202 used as an extracting agent acetonitrile discharge port, the middle part of the recovery tower is provided with a third inlet 201 for recovering the solvent, and the bottom end of the recovery tower is provided with a fifth outlet 203 for discharging heavy components such as 2-ethylnaphthalene and the like;
the dimethylnaphthalene is further concentrated by adopting a lower side line extraction rectifying tower 1, a small amount of light components are discharged from the top of the lower side line extraction rectifying tower 1, high-concentration dimethylnaphthalene is obtained from a lower side line discharge port, the top and bottom pressures of the rectifying tower 1 are respectively controlled to be 0.005MPa and 0.010MPa, the top and bottom temperatures of the rectifying tower 1 are respectively controlled to be 93.4-95.8 ℃ and 176.3-178.7 ℃, the side line temperature of the rectifying tower 1 is 161.2-163.5 ℃ and the reflux ratio is 3:1, under the condition of stable operation, the content of the dimethylnaphthalene reaches 86.76% and the yield reaches 95.72% in the side line discharge of the lower side line extraction rectifying tower 1.
The pressure at the top and the bottom of the solvent recovery tower 2 are respectively controlled to be 0.1MPa and 0.105MPa, the temperature at the top and the bottom of the recovery tower 2 are respectively 80.1-82.5 ℃ and 253.2-255.6 ℃, the reflux ratio is 2, the extractant in the discharged material at the top of the tower is recycled, the content of the extractant in the solvent recovery tower T2 reaches 99.98 percent and the yield reaches 99.94 percent under the condition of stable operation.
TABLE 1 Process conditions for the separation Process
TABLE 2 results of concentrating dimethylnaphthalenes in catalytically cracked light cycle oil LCO
Application example 2: by using the device in example 1, the residual fractions with the mass content of the dimethylnaphthalene of 62.45%, the mass content of the 2-ethylnaphthalene of 16.85% and the mass content of the trimethylnaphthalene of 5.99% are used as raw materials, the dimethylnaphthalene is further concentrated by using the rectifying tower 1, a small amount of light components are discharged from the top of the rectifying tower 1, the high-concentration dimethylnaphthalene is obtained from a lower side discharge port, the top and bottom pressures of the rectifying tower 1 are controlled to be 0.005MPa and 0.010MPa respectively, the top and bottom temperatures of the rectifying tower 1 are respectively 93.4-95.8 ℃ and 176.3-178.7 ℃, the side temperature of the rectifying tower 1 is 161.2-163.5 ℃ and the ratio is 4:1, and under the condition of stable operation, the content of the dimethylnaphthalene in the side discharge of the rectifying tower 1 reaches 87.16% and the yield reaches 96.21%. The top discharge of the rectifying tower 1 is treated by a recovery tower 2 for solvent recovery, the bottom fraction of the recovery tower 2 is used as C10 solvent oil, the top extractant can be recycled, the top and bottom pressures of the recovery tower 2 are controlled to be 0.1MPa and 0.105MPa respectively, the top and bottom temperatures of the recovery tower 2 are controlled to be 80.1-82.5 ℃ and 253.2-255.6 ℃ respectively, the reflux ratio is 2, the extractant in the top discharge of the recovery tower 2 is recycled, the content of the extractant in the recovery tower 2 reaches 99.98% and the yield reaches 99.94% under the condition of stable operation.
Application example 3:
by using the device in the embodiment 1, the residual fractions with the mass content of the dimethylnaphthalene of 62.45%, the mass content of the 2-ethylnaphthalene of 16.85% and the mass content of the trimethylnaphthalene of 5.99% are used as raw materials, the dimethylnaphthalene is further concentrated by using the rectifying tower 1, a small amount of light components are discharged from the top of the rectifying tower 1, the high-concentration dimethylnaphthalene is obtained from a lower side discharge port, the top and bottom pressures of the rectifying tower 1 are respectively controlled to be 0.005MPa and 0.010MPa, the temperatures of the top and bottom of the rectifying tower are respectively 93.4-95.8 ℃ and 176.3-178.7 ℃, the side temperature is 161.2-163.5 ℃ and the reflux ratio is 5:1, and under the condition of stable operation, the content of the dimethylnaphthalene in the side discharge of the rectifying tower 1 reaches 87.86%, and the yield reaches 96.75%. The material discharged from the top of the rectifying tower 1 is treated by a recovery tower 2, and the fraction at the bottom of the recovery tower 2 is used as C10The solvent oil is used, the extractant at the top of the tower can be recycled, the pressure at the bottom of the top of the recovery tower 2 is controlled to be 0.1MPa and 0.105MPa respectively, the temperature at the top and the bottom of the recovery tower 2 are controlled to be 80.1-82.5 ℃ and 253.2-255.6 ℃ respectively, the reflux ratio is 2, the extractant in the discharged material at the top of the tower is recycled, under the condition of stable operation, the content of the extractant in the solvent recovery tower T2 reaches 99.98%, and the yield reaches 99.94%.
Claims (5)
1. The method for concentrating dimethylnaphthalene by extractive distillation is characterized by comprising the following steps:
(a) taking residual fractions with the mass content of 62.45% of dimethylnaphthalene, 16.85% of 2-ethylnaphthalene and 5.99% of trimethylnaphthalene as raw materials, wherein a rectifying tower (1) comprises a first inlet (101) for raw materials to enter, a second inlet (102) for an extracting agent to enter, a first outlet (103) arranged at the bottom end of the rectifying tower (1), a second outlet (104) arranged at the top end of the rectifying tower (1) and a third outlet (105) arranged at the side edge of the rectifying tower (1); the method comprises the following steps that raw materials enter a rectifying tower (1) from a first inlet (101) of the rectifying tower (1), an extracting agent is introduced from a second inlet (102), the pressure of the top and the bottom of the rectifying tower (1) is controlled to be 0.005MPa, the pressure of the bottom of the rectifying tower (1) is controlled to be 0.010MPa, and the reflux ratio is 3-5: 1; the top temperature of the rectifying tower (1) is 93.4-95.8 ℃, the side temperature of the rectifying tower (1) is 161.2-163.5 ℃, and the bottom temperature of the rectifying tower (1) is 176.3-178.7 ℃; the extractant is acetonitrile; the rectifying tower (1) is a lower side line extraction rectifying tower;
(b) the recovery tower (2) is provided with a third inlet (201) communicated with the second outlet (104), a fourth outlet (202) which is arranged at the top end of the recovery tower (2) and communicated with the second inlet (102), and a fifth outlet (203) which is arranged at the bottom end of the recovery tower (2); and (3) introducing an extracting agent from a third inlet (201) of the recovery tower (2), controlling the pressure at the top of the recovery tower (2) to be 0.1-0.105 MPa, the pressure at the bottom of the recovery tower (2) to be 0.105-0.115 MPa, the temperature at the top of the recovery tower (2) to be 80.1-82.5 ℃, and the temperature at the bottom of the recovery tower (2) to be 253.2-255.6 ℃.
2. The method for the concentration of dimethylnaphthalene by extractive distillation according to claim 1, wherein a collecting tank (3) is arranged at the third outlet (105) of the distillation column (1), a plurality of steam guide pipes (301) and overflow pipes (302) are distributed in the collecting tank (3), the steam guide pipes and the overflow pipes are uniformly distributed in a crossed manner, and the bottom of the collecting tank (3) is connected with a side-stream discharge hole (303).
3. The method for the concentration by extractive distillation of dimethylnaphthalene according to claim 1, wherein in step (a), the number of theoretical plates of the distillation column (1) is 90 to 110.
4. The method for the extractive distillation concentration of dimethylnaphthalene according to claim 2, characterized in that the first inlet (101) is higher than the second inlet (102).
5. The method for the extractive distillation concentration of dimethylnaphthalene according to claim 2, wherein the height of the third outlet (105) is lower than the height of the second inlet (102).
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1541988A (en) * | 2003-04-29 | 2004-11-03 | 中国石油化工股份有限公司 | Method for separating arene by extraction and rectification |
| CN202554988U (en) * | 2012-04-05 | 2012-11-28 | 南京师范大学 | Decompressing rectifying lateral line discharged material collection device |
| CN206518910U (en) * | 2017-01-20 | 2017-09-26 | 南京师范大学 | One kind extraction lateral line discharging rectifier unit |
| CN207076152U (en) * | 2017-07-17 | 2018-03-09 | 江苏五洋碳氢科技有限公司 | The lower lateral line discharging rectifier unit of one kind extraction |
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- 2019-10-09 CN CN201910954305.9A patent/CN110759804B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1541988A (en) * | 2003-04-29 | 2004-11-03 | 中国石油化工股份有限公司 | Method for separating arene by extraction and rectification |
| CN202554988U (en) * | 2012-04-05 | 2012-11-28 | 南京师范大学 | Decompressing rectifying lateral line discharged material collection device |
| CN206518910U (en) * | 2017-01-20 | 2017-09-26 | 南京师范大学 | One kind extraction lateral line discharging rectifier unit |
| CN207076152U (en) * | 2017-07-17 | 2018-03-09 | 江苏五洋碳氢科技有限公司 | The lower lateral line discharging rectifier unit of one kind extraction |
Non-Patent Citations (2)
| Title |
|---|
| Purification of 2,6-dimethylnaphthalene containing in light cycle oil by distillation-solvent extraction-solute crystallization combination;Su Jin Kim;《Journal of Industrial and Engineering Chemistry》;20190621;第79卷;第146-153页 * |
| Separation and Recovery of Dimethylnaphthalene Isomers from Light Cycle Oil by Distillation-Extraction Combination;Su Jin Kim等;《Separation Science and Technology》;20031231;第38卷(第16期);第4095-4116页 * |
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