CN107628930B - Energy-saving process for separating methanol, isopropanol and water by heat pump extractive distillation - Google Patents
Energy-saving process for separating methanol, isopropanol and water by heat pump extractive distillation Download PDFInfo
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- CN107628930B CN107628930B CN201710977234.5A CN201710977234A CN107628930B CN 107628930 B CN107628930 B CN 107628930B CN 201710977234 A CN201710977234 A CN 201710977234A CN 107628930 B CN107628930 B CN 107628930B
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Abstract
The invention provides an energy-saving process for separating methanol, isopropanol and water by heat pump extractive distillation. In the method for separating the methanol-isopropanol-water mixture by the heat pump extractive distillation, the steam at the top of a dehydrating tower is pressurized by a heat pump compressor and then is used as a heat source at the bottom of an isopropanol removal tower, and the steam at the top of the dehydrating tower is condensed; the hot extractant flow recovered from the bottom of the dehydrating tower is used as the heat source of the intermediate reboiler of the methanol removing tower. The temperature and the pressure of the steam at the top of the dehydrating tower are properly improved by the heat pump compressor and are used as a heat source to heat the kettle liquid, so that reasonable and effective energy circulation is realized; the cost generated by the heat pump compressor is lower than that of the traditional external heat supply and cooling water, and good economic benefit is generated.
Description
[ technical field ] A method for producing a semiconductor device
The invention belongs to the field of separation and purification in the chemical industry, and particularly relates to a process for separating methanol-isopropanol-water by heat pump extractive distillation.
[ background of the invention ]
Methanol (methanol) and isopropanol (isopropanol) are important organic chemicals and solvents. Methanol is mainly used for manufacturing medicines, pesticides, formaldehyde, organic glass and the like, and is also a solvent for paint dyes, nitrocellulose and the like. The isopropanol can be used as raw materials for producing acetone, hydrogen peroxide, methyl isobutyl ketone, medicines, pesticides and the like, and can be used for producing solvents and the like in the production of coatings, printing inks, extracting agents, aerosol and the like. In the production of pharmaceutical factories, a large amount of methanol-isopropanol-water mixture is generated, and the separation of the methanol-isopropanol-water mixture has great economic benefit for enterprises. But the isopropanol and the water form an azeotrope under normal pressure, the azeotropic temperature is 80.18 ℃, the azeotropic composition is 12.1 percent of water, and the purity requirement cannot be met by common rectification.
Chinese patent CN 103588620A discloses a method for separating isopropanol-water azeotrope by extractive distillation, which takes ionic liquid as an extracting agent, operates in a single tower, and has the advantages of high product purity and easy control. However, this method has the disadvantages of small throughput, and large energy consumption because it cannot be operated continuously for batch operation.
Chinese patent CN 103819302A discloses a method for separating a mixture of toluene, methanol, isopropanol and dimethyl carbonate, the mixture is separated by organic solvent extraction and rectification, the product purity is high, the separation cost is low, the method relates to the separation of methanol and isopropanol, and a methanol-isopropanol-water ternary system is not involved.
Chinese patent CN 101391152A discloses a method for separating an ethanol-water azeotrope, which not only minimizes the energy consumption of batch rectification and optimizes the use way of heat by controlling a heat pump, but also improves the yield of ethanol by extracting batch rectification and reduces the difficulty of tower bottom liquid recovery. However, this method cannot realize continuous production.
[ summary of the invention ]
[ problem to be solved ]
The invention aims to provide a method for extracting and rectifying a methanol-isopropanol-water mixture by a heat pump, which solves the problem that the methanol-isopropanol-water mixture is difficult to separate due to azeotropy, realizes high-efficiency separation and heat energy integration of methanol, isopropanol and water, and realizes the purpose of energy conservation.
[ solution ]
The invention is realized by the following technical scheme.
An energy-saving process for separating methanol, isopropanol and water by adopting heat pump extractive distillation comprises the following steps:
(1) introducing a mixture of methanol, isopropanol and water into a methanol removing tower (T1) through a pipeline 1, wherein one stream in the middle of the methanol removing tower (T1) passes through an intermediate reboiler (R2) and then returns to the methanol removing tower (T1), a heat source of the intermediate reboiler (R2) is provided by a hot stream at the bottom of a dehydrating tower (T3), steam at the top of the methanol removing tower (T1) sequentially passes through a condenser (C1) for condensation and a reflux tank (D1) for collection, one part of the condensed steam returns to the top of the methanol removing tower (T1), the other part of the top of the tower is taken out as a methanol product through a pipeline 4, one part of the material at the bottom of the methanol removing tower (T1) enters a reboiler (R1), the vaporized material returns to the bottom of the methanol removing tower (T1), and the other part of the material at the bottom of the tower enters an isopropanol;
(2) the top steam of the isopropanol removal tower (T2) passes through a condenser (C2) and a reflux tank (D2) in sequence through a pipeline 9, a part of the condensed steam returns to the isopropanol removal tower (T2), and a part of the condensed steam is extracted through a pipeline 3. The bottom stream of the isopropanol removal tower (T2) enters a reboiler (R3) through a pipeline 12, the heat source of the reboiler (R3) is provided by steam which is pressurized by a heat pump compressor (P1) through a dehydration tower (T3), and the steam flows into a flash tank (F1) through a pipeline 14 after being heated;
(3) the top steam of the flash tank (F1) enters the bottom of an isopropanol removal tower (T2), and the bottom liquid of the flash tank (F1) enters a dehydration tower (T3) through a pipeline 16;
(4) the steam at the top of the dehydrating tower (T3) is pressurized and heated by a heat pump (P1) to be used as a heat source of a reboiler (R3), and flows into a splitter (S1) after being subjected to heat exchange with the bottom stream of the isopropanol removal tower (T2), one part of the steam returns to the top of the dehydrating tower (T3) through a pipeline 18, and the other part of the steam is extracted through a pipeline 17;
an energy-saving process for separating methanol, isopropanol and water by heat pump extractive distillation is characterized in that a methanol removing tower (T1) is a normal pressure tower, the number of theoretical plates is 57-62, the feeding position is 23-27, the material flow connecting position of an intermediate reboiler is 49-52 plates, and the reflux ratio of the methanol removing tower (T1) is 8-10; the operation pressure of the isopropanol removal tower (T2) is 0.5atm, the number of theoretical plates is 37-42, the mass solvent ratio is 1-1.3, the feeding position of the extracting agent is 2-4 th plates, the position of the mixture feeding plate is 28-31, and the reflux ratio of the isopropanol removal tower (T2) is 1-3; the number of theoretical plates of the atmospheric dehydration tower (T3) is 18-24, the position of a feed plate is 9-13, and the split ratio of a splitter (S1) is 0.55-0.63; the temperature of the top of the methanol removing tower (T1) is 64.52-65.03 ℃, the temperature of the bottom of the methanol removing tower is 89.05-89.31 ℃, the temperature of the top of the isopropanol removing tower (T2) is 65.55-66.08 ℃, the temperature of the bottom of the methanol removing tower is 100.02-100.51 ℃, the temperature of the top of the dehydrating tower (T3) is 100.01-100.15 ℃, and the temperature of the bottom of the dehydrating tower is 200.01-201.60 ℃.
An energy-saving process for separating methanol, isopropanol and water by heat pump extractive distillation is characterized in that the mass fraction of methanol obtained from the top of a methanol removing tower (T1) is more than 99.96%, the recovery rate of methanol is more than 99.85%, the mass fraction of isopropanol obtained from the top of an isopropanol removing tower (T2) is more than 99.90%, the recovery rate of isopropanol is more than 99.75%, the mass fraction of water obtained from the top of a dehydrating tower (T3) is more than 99.90%, and the dehydration rate is more than 99.95%.
An energy-saving process for separating methanol, isopropanol and water by using heat pump extractive distillation is characterized in that a hot stream at the bottom of a dehydration tower (T3) is used as a heat source of an intermediate reboiler of a methanol removing tower (T1) and is thermally integrated with the methanol removing tower (T1).
An energy-saving process for separating methanol, isopropanol and water by heat pump extractive distillation is characterized in that a steam material flow at the top of a dehydrating tower (T3) is subjected to pressure boosting and temperature rising by a heat pump (P1) to be used as a heat source of a tower bottom reboiler (R3) of a deisopropanol tower (T2) to exchange heat with liquid at the bottom of the deisopropanol tower (T2), after heat exchange, steam at the top of the tower is condensed into liquid, the liquid is divided into two material flows by a flow divider (S1), one material flow is taken as an aquatic product to be extracted, and the other material flow flows back to the top of the dehydrating tower (T3.
An energy-saving process for separating methanol, isopropanol and water by heat pump extractive distillation is characterized in that an extractant used by an isopropanol removal tower (T2) is ethylene glycol.
An energy-saving process for separating methanol, isopropanol and water by extraction and rectification of a heat pump is characterized in that an extracting agent recovered from the bottom of a dehydration tower (T3) enters an isopropanol removal tower (T2) for cyclic utilization after heat exchange is completed in an intermediate reboiler of the methanol removal tower.
The energy-saving process for separating methanol, isopropanol and water by heat pump extractive distillation realizes that the purity of the methanol, the isopropanol and the water is more than 99.90 percent.
[ description of the drawings ]
FIG. 1 is a schematic diagram of an energy-saving process for separating methanol-isopropanol-water by extractive distillation with a heat pump.
In the figure: t1 — a demethanizer; t2-isopropanol removal tower; t3 — dehydration column; r1, R3, R3-bottom reboiler; r2 — intermediate reboiler; f1-flash tank; s1-a splitter; c1, C2-overhead condenser; d1, D2-reflux drum; p1 — heat pump; the numbers represent the respective lines.
The invention is further described below in conjunction with the accompanying fig. 1 and the detailed description, but is not limited to the drawings and the implementation.
[ advantageous effects ]
Compared with the prior art, the invention mainly has the following beneficial effects:
(1) the method successfully separates the methanol-isopropanol-water mixture, has high product purity, safe process, environmental protection and no pollution, and can realize clean production. Solves the problem that the methanol-isopropanol-water mixture is difficult to separate azeotropically.
(2) The invention adopts thermal coupling and heat pump technology, fully and effectively utilizes heat energy, and reduces energy consumption in the extraction and rectification process.
(3) The invention realizes the effective recycling of the extracting agent.
[ detailed description ] embodiments
The present invention will be further described with reference to the following examples, but the present invention is not limited to these examples.
Example 1:
2000kg/h of a 20 wt.% aqueous solution of methanol and 30 wt.% isopropanol are used as examples:
the number of trays in the demethanizer (T1) was 60, the mixed feed entered the demethanizer (T1) from the 25 th tray, and stream 6 was refluxed to the demethanizer (T1) from the 50 th tray after heat exchange with the bottoms of the intermediate reboiler (R2) and the dehydration column (T3). The bottom stream 5 of the demethanizer (T1) was fed from the 30 th column to the deisopropanizer (T2), the deisopropanizer (T2) had a total of 42 trays, and the extractant ethylene glycol was fed from the 2 nd tray to the deisopropanizer (T2), with an extractant ethylene glycol flow rate of 2000 kg/h. The operating pressure of the dehydration column was atmospheric and the dehydration column (T3) had a total of 22 plates. The mixed solution of water and extractant is introduced into the dehydration column (T3) from the 12 th plate of the dehydration column (T3). The temperature at the top of the demethanizer (T1) was 64.54 ℃ and the temperature at the bottom of the demethanizer was 89.05 ℃. The temperature at the top of the deisopropanol column (T2) was 65.60 ℃ and the temperature at the bottom of the deisopropanol column was 100.30 ℃. The temperature at the top of the dehydration column (T3) was 100.10 ℃ and the temperature at the bottom of the column was 201.61 ℃. Methanol with the purity of 99.99 percent is obtained from the methanol removing tower (T1), isopropanol removing tower (T2) obtains isopropanol with the purity of 99.6 percent, and pure extractant is recovered from the bottom of the dehydrating tower (T3). The temperature of the outlet steam at the top of the dehydrating tower (T3) after being compressed by a heat pump is 226.60 ℃, and the pressure is 2.5 bar. The separation ratio of the splitter (S1) was 0.59.
Example 2:
take 1800kg/h of a 17 wt% methanol and 33 wt% isopropanol mixed solution as an example:
the number of trays in the demethanizer (T1) was 58, the mixed feed entered the demethanizer (T1) from tray 24, and stream 6 was refluxed to the demethanizer (T1) from tray 51 after heat exchange with the bottoms of the intermediate reboiler (R2) and the dehydration column (T3). The bottom stream 5 of the demethanizer (T1) was taken from the 31 st column to the deisopropanizer (T2), the deisopropanizer (T2) had 41 trays, and the extractant ethylene glycol was taken from the 4 th tray to the deisopropanizer (T2), at an extractant ethylene glycol flow rate of 1850 kg/h. The operating pressure of the dehydration column was atmospheric and the dehydration column (T3) had a total of 23 plates. The mixed solution of water and extractant is introduced into the dehydration column (T3) from the 12 th plate of the dehydration column (T3). The temperature of the top of the demethanizer (T1) was 64.52 ℃ and the temperature of the bottom of the demethanizer was 89.08 ℃. The temperature at the top of the deisopropanol column (T2) was 65.89 ℃ and the temperature at the bottom of the deisopropanol column was 100.40 ℃. The temperature at the top of the dehydration column (T3) was 100.10 ℃ and the temperature at the bottom of the column was 201.60 ℃. Methanol with the purity of 99.99 percent is obtained from the methanol removing tower (T1), isopropanol removing tower (T2) obtains isopropanol with the purity of 99.6 percent, and pure extractant is recovered from the bottom of the dehydrating tower (T3). The temperature of the outlet steam at the top of the dehydrating tower (T3) after being compressed by a heat pump is 226.58 ℃, and the pressure is 2.5 bar. The separation ratio of the splitter (S1) was 0.60.
Example 3:
taking 2100kg/h of a mixed solution of 22 wt% methanol and 32 wt% isopropanol as an example:
the number of trays in the demethanizer (T1) was 61, the mixed material entered the demethanizer (T1) from the 26 th tray, and stream 6 was refluxed to the demethanizer (T1) from the 49 th tray after heat exchange with the bottoms of the intermediate reboiler (R2) and the dehydration column (T3). The bottom stream 5 of the methanol removing tower (T1) enters an isopropanol removing tower (T2) from a 28 th tower, the isopropanol removing tower (T2) has 42 trays, the extractant glycol enters the isopropanol removing tower (T2) from a 3 rd tray, and the flow rate of the extractant glycol is 2050 kg/h. The operating pressure of the dehydration column was atmospheric and the dehydration column (T3) had a total of 20 plates. The mixed solution of water and extractant is introduced into the dehydration column (T3) from the 13 th plate of the dehydration column (T3). The temperature at the top of the demethanizer (T1) was 65.03 ℃ and the temperature at the bottom of the demethanizer was 89.08 ℃. The temperature at the top of the deisopropanol column (T2) was 65.59 ℃ and the temperature at the bottom of the deisopropanol column was 100.41 ℃. The temperature at the top of the dehydration column (T3) was 100.02 ℃ and the temperature at the bottom of the column was 200.47 ℃. Methanol with the purity of 99.99 percent is obtained from the methanol removing tower (T1), isopropanol removing tower (T2) obtains isopropanol with the purity of 99.6 percent, and pure extractant is recovered from the bottom of the dehydrating tower (T3). The temperature of the outlet steam at the top of the dehydrating tower (T3) after being compressed by a heat pump is 226.49 ℃, and the pressure is 2.5 bar. The split ratio of the splitter (S1) was 0.57.
Example 4:
take 2050kg/h of a 23 wt% methanol and 28 wt% isopropanol mixed solution as an example:
the number of trays in the demethanizer (T1) was 62, the mixed feed entered the demethanizer (T1) from tray 23, and stream 6 was refluxed to the demethanizer (T1) from tray 52 after heat exchange with the bottoms of the intermediate reboiler (R2) and the dehydration column (T3). The bottom stream 5 of the methanol removing tower (T1) enters an isopropanol removing tower (T2) from a 28 th tower, the isopropanol removing tower (T2) has 39 tower plates in total, the extractant glycol enters the isopropanol removing tower (T2) from a 4 th plate, and the flow rate of the extractant glycol is 2050 kg/h. The operating pressure of the dehydration column was atmospheric and the dehydration column (T3) had a total of 19 plates. The mixed solution of water and extractant is introduced into the dehydration column (T3) from the 9 th plate of the dehydration column (T3). The temperature of the top of the demethanizer (T1) was 64.55 ℃ and the temperature of the bottom of the demethanizer was 89.31 ℃. The temperature at the top of the isopropanol removal column (T2) was 66.01 ℃ and the temperature at the bottom of the column was 100.10 ℃. The temperature at the top of the dehydration column (T3) was 100.05 ℃ and the temperature at the bottom of the column was 200.87 ℃. Methanol with the purity of 99.99 percent is obtained from the methanol removing tower (T1), isopropanol removing tower (T2) obtains isopropanol with the purity of 99.6 percent, and pure extractant is recovered from the bottom of the dehydrating tower (T3). The temperature of the outlet steam at the top of the dehydrating tower (T3) after being compressed by a heat pump is 226.60 ℃, and the pressure is 2.5 bar. The separation ratio of the splitter (S1) was 0.6.
Claims (3)
1. An energy-saving process for separating methanol, isopropanol and water by heat pump extractive distillation is characterized in that a heat pump distillation method and a device used by the process comprise the following parts:
a methanol removing tower (T1), an isopropanol removing tower (T2), a dehydrating tower (T3), a reboiler (R1), an intermediate reboiler (R2), a reboiler (R3), a reboiler (R4), a reflux tank (D1), a reflux tank (D2), a flow divider (S1), a condenser (C1), a condenser (C2), a flash tank (F1) and a heat pump compressor (P1), wherein the intermediate reboiler (R2) is connected to the middle section of the methanol removing tower, the reboiler (R1), the reboiler (R3) and the reboiler (R4) are respectively connected to the bottoms of the methanol removing tower (T1), the isopropanol removing tower (T2) and the dehydrating tower (T3), the condenser (C1) and the reflux tank (D1) are sequentially connected to the top of the methanol removing tower through pipelines, the condenser (C2) and the reflux tank (D2) are sequentially connected to the top of the isopropanol removing tower, and the splitter (S1) and the heat pump compressor (P1) are sequentially connected to the top of the dehydrating tower through pipelines;
the extractant used by the isopropanol removal tower (T2) is ethylene glycol;
the process mainly comprises the following steps:
(1) introducing a mixture of methanol, isopropanol and water into a methanol removing tower (T1) through a pipeline 1, wherein one stream in the middle of the methanol removing tower (T1) passes through an intermediate reboiler (R2) and then returns to the methanol removing tower (T1), a heat source of the intermediate reboiler (R2) is provided by a hot stream at the bottom of a dehydrating tower (T3), steam at the top of the methanol removing tower (T1) sequentially passes through a condenser (C1) for condensation and a reflux tank (D1) for collection, one part of the condensed steam returns to the top of the methanol removing tower (T1), the other part of the top of the tower is taken out as a methanol product through a pipeline 4, one part of the material at the bottom of the methanol removing tower (T1) enters a reboiler (R1), the vaporized material returns to the bottom of the methanol removing tower (T1), and the other part of the material at the bottom of the tower enters an isopropanol;
(2) the top steam of the isopropanol removal tower T2 sequentially passes through a condenser (C2) and a reflux tank (D2) through a pipeline 9, a part of condensed steam returns to the isopropanol removal tower (T2), a part of condensed steam is extracted through a pipeline 3, the bottom stream of the isopropanol removal tower (T2) enters a reboiler (R3) through a pipeline 12, the heat source of the reboiler (R3) is provided by a dehydration tower (T3) and steam pressurized by a heat pump compressor (P1), and the heated steam flows into a flash tank (F1) through a pipeline 14;
(3) the top steam of the flash tank (F1) enters the bottom of an isopropanol removal tower (T2), and the bottom liquid of the flash tank (F1) enters a dehydration tower (T3) through a pipeline 16;
(4) the steam at the top of the dehydrating tower (T3) is used as a heat source of a reboiler (R3) after being pressurized and heated by a heat pump (P1), and flows into a flow divider (S1) after being subjected to heat exchange with the bottom stream of the isopropanol removal tower (T2), one part of the steam returns to the top of the dehydrating tower (T3) through a pipeline 18, the extractant recovered at the bottom of the dehydrating tower (T3) enters the isopropanol removal tower (T2) for recycling after the heat exchange is completed by the middle reboiler of the isopropanol removal tower, and the other part of the steam is extracted through a pipeline 17.
2. The process according to claim 1, characterized in that: the methanol removing tower (T1) is an atmospheric tower, the number of theoretical plates is 57-62, the feeding position is 23-27, the intermediate reboiler material flow connecting position is 49-52 plates, and the reflux ratio of the methanol removing tower (T1) is 8-10; the operation pressure of the isopropanol removal tower (T2) is 0.5atm, the number of theoretical plates is 37-42, the mass solvent ratio is 1-1.3, the feeding position of the extracting agent is 2-4, the position of the mixture feeding plate is 28-31, and the reflux ratio of the isopropanol removal tower (T2) is 1-3; the number of theoretical plates of the atmospheric dehydration tower (T3) is 18-24, the position of a feed plate is 9-13, and the split ratio of a splitter (S1) is 0.55-0.63; the temperature of the top of the methanol removing tower (T1) is 64.52-65.03 ℃, the temperature of the bottom of the methanol removing tower is 89.05-89.31 ℃, the temperature of the top of the isopropanol removing tower (T2) is 65.55-66.08 ℃, the temperature of the bottom of the methanol removing tower is 100.02-100.51 ℃, the temperature of the top of the dehydrating tower (T3) is 100.01-100.15 ℃, and the temperature of the bottom of the dehydrating tower is 200.01-201.60 ℃.
3. The process according to claim 1, characterized in that: the mass fraction of the methanol obtained from the top of the methanol removing tower (T1) is more than 99.96 percent, the recovery rate of the methanol is more than 99.85 percent, the mass fraction of the isopropanol obtained from the top of the isopropanol removing tower (T2) is more than 99.90 percent, the recovery rate of the isopropanol is more than 99.75 percent, the mass fraction of the water obtained from the top of the dehydrating tower (T3) is more than 99.90 percent, and the dehydration rate is more than 99.95 percent.
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| CN111792998A (en) * | 2020-06-30 | 2020-10-20 | 北京诺维新材科技有限公司 | Method for separating methylamine |
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| CN112125802B (en) * | 2020-09-29 | 2021-07-09 | 中国石油大学胜利学院 | Extractive distillation separation system and method for ethyl acetate-isopropanol-water mixture |
| CN112479800B (en) * | 2020-12-10 | 2023-06-16 | 常州瑞华化工工程技术股份有限公司 | Energy-saving process for recycling propylene |
| CN113788740B (en) * | 2021-09-17 | 2024-03-29 | 天津大学 | Method for recovering methanol and ethanol from fusel oil containing water |
| CN115340443A (en) * | 2022-08-03 | 2022-11-15 | 青岛科技大学 | Method for separating isopropanol-water-ethanol mixture by thermal coupling extractive distillation |
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| 正丙醇-异丙醇-水共沸体系分离工艺模拟;王桂英等;《吉林化工学院学报》;20170515;第34卷(第5期);第1页1.2部分，第2页右栏，图3 * |
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