CN115710166B - Rectification process for separating isopropanol-diisopropyl ether-water mixture - Google Patents

Rectification process for separating isopropanol-diisopropyl ether-water mixture Download PDF

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CN115710166B
CN115710166B CN202211570017.1A CN202211570017A CN115710166B CN 115710166 B CN115710166 B CN 115710166B CN 202211570017 A CN202211570017 A CN 202211570017A CN 115710166 B CN115710166 B CN 115710166B
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tower
diisopropyl ether
purity
isopropyl alcohol
water
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CN115710166A (en
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孙硕
刘庭蕾
邵晓骐
包可珂
邵琦
任红梅
王勇
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Anhui Enthalpy Valley Engineering Technology Co ltd
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Abstract

The invention relates to the technical field of fine chemical industry, in particular to a rectification process for separating an isopropyl alcohol-diisopropyl ether-water mixture, which adopts ethylene oxide as a reaction extractant, and the isopropyl alcohol-diisopropyl ether-water mixture is pre-concentrated through a pre-concentration tower after heat exchange with materials extracted from the bottoms of a tower T1 and a tower T3, the isopropyl alcohol-diisopropyl ether-water mixture with low water content is separated, then the isopropyl alcohol-diisopropyl ether-water mixture and the ethylene oxide are subjected to reaction extractive rectification through a tower T2, high-purity diisopropyl ether is separated from the top of the tower, isopropyl alcohol, ethylene glycol, trace water and ethylene oxide are separated from the bottom of the tower, and finally the high-purity isopropyl ether is obtained through the separation of the tower T3.

Description

Rectification process for separating isopropanol-diisopropyl ether-water mixture
Technical Field
The invention relates to the technical field of fine chemical engineering, in particular to a rectification process for separating an isopropanol-diisopropyl ether-water mixture.
Background
The production of isopropanol takes propylene and water as raw materials, and the isopropanol is produced by hydration with an acidic or cation exchange resin catalyst. During the production of isopropyl alcohol, a large amount of by-products containing diisopropyl ether are obtained. The isopropyl alcohol, diisopropyl ether and water form a ternary azeotrope under normal pressure, the azeotropic temperature is 61.8 ℃, the azeotropic composition is 4.0 percent (wt%) of isopropyl alcohol, 91.0 percent of diisopropyl ether and 5.0 percent of water, the minimum azeotrope is formed between the two components, and a high-purity product cannot be obtained by a conventional rectification method.
The rectification separation technology is mature and easy to industrialize, but has the defect of high energy consumption. In conventional rectification separation, the input energy consumption is more than 40% of the total industrial energy consumption, which is not negligible in the 21 st century when the energy source is increasingly scarce, in a conventional rectification column, the energy introduced into the reboiler of the rectification column is discharged through a condenser, most of the energy is lost in terms of pressure drop such as column and temperature difference through a heat exchanger, and only part of the energy is used to reduce the entropy of the product. Rather than discharging all the heat from the tower to the atmosphere, the energy level is not increased to be utilized, so that the consumption of reboiling steam is reduced or eliminated, and the energy-saving effect is achieved.
U.S. patent No. 06069284 discloses a process for separating diisopropyl ether from a mixture of diisopropyl ether, isopropanol and water by first distilling the mixture in a distillation column into a bottom stream containing water and isopropanol and a top stream containing an azeotrope of diisopropyl ether, isopropanol and water, the top stream being condensed and allowing to form in a top receiver an aqueous phase rich in isopropanol and water and an organic phase rich in diisopropyl ether and some water and isopropanol, the aqueous phase being recycled to the distillation column, the organic phase being passed to a dryer to form a bottom product stream containing at least 99 mole% diisopropyl ether and a top stream containing an azeotrope of diisopropyl ether, isopropanol and water, condensing and introducing the drier top stream into the top receiver to combine with the condensed stream from the distillation column and form the aqueous and organic phases described above, collecting the diisopropyl ether product from the bottom of the dryer, but the process is only capable of processing mixtures of diisopropyl ether, isopropanol and water in a water content of around 20% and complex and the obtained product is only capable of achieving a high energy consumption of 95% and a high energy consumption of the product.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a rectification process for separating an isopropyl alcohol-diisopropyl ether-water mixture, which combines a three-tower process with a pre-concentration tower with a heat integration technology, improves the purity of products, reduces energy consumption and environmental emission and improves thermodynamic efficiency compared with the design of a conventional extraction rectification process.
In order to solve the above problems, the present invention provides a rectification process for separating an isopropyl alcohol-diisopropyl ether-water mixture, wherein the process comprises a three-tower mode, a tower T1 is a simple preconcentration tower which is conventional in the art, a tower T2 is a reactive extraction rectification tower, a tower T3 is a common rectification tower, and the specific rectification process steps are as follows:
(1) After heat exchange is carried out on the mixture containing isopropyl alcohol-diisopropyl ether-water and tower bottom produced materials of the tower T1 and the tower T3, the mixture enters the tower T1 from the middle part of the tower T1, the mixture is pre-concentrated, diisopropyl ether, isopropyl alcohol and water are produced from the tower top, the mixture enters the tower T2, and high-purity water is produced from the tower bottom;
(2) Ethylene oxide enters a tower T2 from the middle part of the tower T2, reacts and separates with components from the tower T1 and the tower T3 in the tower T2, high-purity diisopropyl ether is extracted from the tower top, isopropanol, ethylene glycol, trace water and ethylene oxide are extracted from the tower bottom, and the mixture enters the tower T3;
(3) The components from the tower T2 are separated in a tower T3, high-purity isopropanol is separated from the tower top, high-purity ethylene glycol is extracted from the tower bottom, part of the high-purity ethylene glycol is cooled and then enters the tower T2 for circulation, and the rest of the high-purity ethylene glycol is extracted.
Preferably, the operating pressure of the tower T1 is 101kPa, the top temperature is 60-63 ℃, the bottom temperature is 102-106 ℃, the theoretical plate number is 14-20, the reflux ratio is 0.7-0.8, and the feeding position of the mixture of isopropanol-diisopropyl ether-water is 10-13.
Preferably, the operating pressure of the tower T2 is 101kPa, the tower top temperature is 66-70 ℃, the tower bottom temperature is 115-125 ℃, the theoretical plate number is 25-37 plates, the reflux ratio is 1.3-1.7, the feeding position of the component from the tower T1 is 5-7 plates, the feeding position of the component from the tower T3 is 2-4 plates, and the feeding position of the ethylene oxide is 12-14 plates.
Preferably, the operating pressure of the tower T3 is 101kPa, the temperature of the top of the tower is 80-83 ℃, the temperature of the bottom of the tower is 200-205 ℃, the theoretical plate number is 21-27, the reflux ratio is 2.2-2.8, and the feeding position of the components from the tower T2 is 11-15.
Preferably, the mass ratio of the isopropyl alcohol, the diisopropyl ether and the water in the isopropyl alcohol-diisopropyl ether-water mixture is 1:2-4:5-7.
Preferably, the ratio of the flow rates of the ethylene oxide to isopropyl alcohol-diisopropyl ether-water mixture is 5-7:100.
preferably, the purity of the high-purity diisopropyl ether is 99.95-99.98%, the purity of the high-purity isopropyl alcohol is 99.69-99.71%, the purity of the high-purity water is 99.97-99.99%, and the purity of the high-purity ethylene glycol is 99.97-99.99%.
Preferably, the ratio of the flow rates of the high-purity glycol and the extracted high-purity glycol entering the tower T2 is 4:0.6-1.
Compared with the prior art, the invention has the following beneficial effects:
(1) The invention firstly adopts the pre-concentration tower to reduce the water content in the isopropanol-diisopropyl ether-water mixture, then generates the glycol extractant through the reaction of the ethylene oxide and the rest water, and realizes the separation and purification of ternary azeotropic mixture by utilizing the characteristic of different molecular acting forces of glycol on the isopropanol-diisopropyl ether.
(2) In the invention, the reactive extraction rectification process adopts rectification under normal pressure, and compared with the traditional pressure swing rectification, the consumption can be greatly reduced; and secondly, the invention also adopts a heat integration technology for assistance, thereby greatly reducing the consumption of reboiling steam and further reducing the energy consumption.
(3) Compared with the traditional continuous rectification process, the reactive extraction rectification process has a small number of rectification towers, and the proportion of high-purity glycol and extracted high-purity glycol entering the reactive extraction rectification tower, namely the tower T2 circulation, is reasonably controlled, so that the separation difficulty can be effectively reduced, and the purity of the obtained product is high.
(4) The preconcentration tower, namely the tower T1, can process the mixture of diisopropyl ether, isopropanol and water with the water content of more than 50 percent, reduces the water content to below 10 percent through reasonable reflux ratio, greatly reduces the consumption of propylene oxide and saves resources.
Drawings
FIG. 1 is a flow chart of a rectification process for separating an isopropyl alcohol-diisopropyl ether-water mixture in accordance with the present invention.
The marks in the figure: 1. a preconcentration column, i.e. column T1; 2. the reactive extraction rectifying tower is a tower T2; 3. a common rectifying tower, namely a tower T3; 4. a first reboiler; 5. a second reboiler; 6. a third reboiler; 7. a first condenser; 8. a second condenser; 9. a third condenser; 10. a fourth condenser; 11. a first heat exchanger; 12. a second heat exchanger; 101. 102, 103, 104, 105, 106, 107, 108, 109, 110 are all logistic pipelines.
Referring to fig. 1, the rectification process for separating the isopropanol-diisopropyl ether-water mixture provided by the invention has the following working principle: the isopropyl alcohol-diisopropyl ether-water mixture enters the tower T1 from the middle part of the tower T1 after heat exchange is carried out on materials of the isopropyl alcohol-diisopropyl ether-water mixture and the material of the material flow pipelines 102 and 108 through the material flow pipelines 101 and 12, the isopropyl alcohol and the water are produced after the tower top material of the tower T1 passes through the first condenser 7 and enters the tower T2 through the material flow pipeline 103, the high-purity water is produced after the tower bottom material of the tower T1 passes through the first reboiler 4, the ethylene oxide passes through the material flow pipeline 102 and passes through the first heat exchanger 11, the ethylene oxide enters the tower T2 from the middle part of the tower T2 through the material flow pipeline 104, the high-purity diisopropyl ether is produced after the tower top material of the tower T2 passes through the second condenser 8 and passes through the material flow pipeline 105, the isopropyl alcohol, the ethylene glycol, the trace water and the ethylene oxide are produced after the tower bottom material of the tower T2 passes through the second reboiler 5, the high-purity isopropyl alcohol is produced after the tower top material of the tower T3 passes through the third condenser 9, the high-purity isopropyl alcohol is produced after the tower top material of the tower T3 passes through the material flow pipeline 107, the high-purity ethylene glycol is produced after the high-purity ethylene glycol is produced through the high-purity reboiler 6 and passes through the third heat exchanger 110, and the high-purity ethylene glycol is produced after the high-purity ethylene glycol is partially passes through the fourth condenser 110 and passes through the material pipeline 110 and passes through the high-purity pipeline 12, and the high-purity 2 is cooled down part of the tower 12.
The following description of the technical solutions in the embodiments of the present invention will be clear and complete, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. It will be apparent, however, to one skilled in the art that the present invention may be practiced in other embodiments that depart from these specific details.
Example 1
The feed flow rate is 100kg/h, the feed temperature after heat exchange is 78.5 ℃, the feed contains 10% of isopropyl alcohol, 30% of diisopropyl ether and 60% of water, the operating pressure of a tower T1 is 101kPa, the temperature of the top of the tower is 62.3 ℃, the temperature of the bottom of the tower is 104.4 ℃, the theoretical plate number is 17, the reflux ratio is 0.75, the feeding position of the mixture of isopropyl alcohol and diisopropyl ether and water is 12 th, the operating pressure of a tower T2 is 101kPa, the temperature of the top of the tower is 68.1 ℃, the temperature of the bottom of the tower is 120.5 ℃, the theoretical plate number is 31 th, the reflux ratio is 1.5, the feeding position of a component from the tower T1 is 6 th, the feeding position of a component from the tower T3 is 3 rd, the feeding position of ethylene oxide is 13 th, the flow rate of ethylene oxide is 6 kg/h, the operating pressure of the tower T3 is 101kPa, the temperature of the bottom of the tower is 82.1 ℃, the temperature of the bottom of the tower is 202.3 ℃, the theoretical plate number is 24 th, the reflux ratio is 2.5, the feeding position of a component from the tower T2 is 13 th, the high-purity ethylene glycol and the high-purity ethylene glycol which is recycled into the tower T2 is 4:4:4.1.is the following the temperature is the temperature of the temperature: 0.8, the purity of diisopropyl ether after separation is 99.96%, the recovery rate is 99.9%, the purity of isopropanol is 99.71%, the recovery rate is 99.9%, the purity of water is 99.98%, and the recovery rate is 96%.
TABLE 1
Example 2
The feed flow rate is 100kg/h, the feed temperature after heat exchange is 79.3 ℃, the feed contains 10% of isopropanol, 20% of diisopropyl ether and 70% of water, the column T1 operating pressure is 101kPa, the column top temperature is 62.8 ℃, the column bottom temperature is 105.6 ℃, the theoretical plate number is 20, the reflux ratio is 0.78, the mixture of isopropanol and diisopropyl ether and water is fed at 10 th tray, the column T2 operating pressure is 101kPa, the column top temperature is 66.2 ℃, the column bottom temperature is 116.3 ℃, the theoretical plate number is 26 tray, the reflux ratio is 1.3, the feed position of the component from the column T1 is 7 th tray, the feed position of the component from the column T3 is 4 th tray, the feed position of the ethylene oxide is 14 th tray, the flow rate of the ethylene oxide is 7kg/h, the column T3 operating pressure is 101kPa, the column top temperature is 82.5 ℃, the column bottom temperature is 204.3 ℃, the theoretical plate number is 26 tray, the reflux ratio is 2.7, the feed position of the component from the column T2 is 11 th tray, and the ratio of the high purity ethylene glycol and the high purity ethylene glycol which is recycled into the column T2 and the flow rate of the high purity ethylene glycol is 4:4.4.1.the ratio. 0.9, the purity of diisopropyl ether after separation is 99.98%, the recovery rate is 99.9%, the purity of isopropanol is 99.7%, the recovery rate is 99.9%, the purity of water is 99.97%, and the recovery rate is 95%.
TABLE 2
Example 3
The feed flow rate is 100kg/h, the feed temperature after heat exchange is 78.3 ℃, the feed contains 10% of isopropanol, 40% of diisopropyl ether and 50% of water, the operating pressure of a tower T1 is 101kPa, the temperature of the top of the tower is 60.2 ℃, the temperature of the bottom of the tower is 102.5 ℃, the theoretical plate number is 15, the reflux ratio is 0.7, the feeding position of the mixture of isopropanol and diisopropyl ether and water is 13, the operating pressure of a tower T2 is 101kPa, the temperature of the top of the tower is 69.1 ℃, the temperature of the bottom of the tower is 124.3 ℃, the theoretical plate number is 36, the reflux ratio is 1.7, the feeding position of a component from the tower T1 is 5 th, the feeding position of a component from the tower T3 is 2 nd, the feeding position of ethylene oxide is 12 th, the flow rate of ethylene oxide is 5 kg/h, the operating pressure of the tower T3 is 101kPa, the temperature is 80.3 ℃, the temperature of the bottom of the tower is 201.8 ℃, the theoretical plate number is 22 th, the reflux ratio is 2.3, the feeding position of the component from the tower T2 is 12 th, and the ratio of high-purity ethylene glycol and the flow rate of the high-purity ethylene glycol which is 4. 0.6, the purity of diisopropyl ether after separation is 99.95%, the recovery rate is 99.9%, the purity of isopropanol is 99.69%, the recovery rate is 99.9%, the purity of water is 99.99%, and the recovery rate is 96%.
TABLE 3 Table 3
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential characteristics thereof. The present embodiments are, therefore, to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Furthermore, it should be understood that although the present disclosure describes embodiments, not every embodiment is provided with a separate embodiment, and that this description is provided for clarity only, and that the disclosure is not limited to the embodiments described in detail below, and that the embodiments described in the examples may be combined as appropriate to form other embodiments that will be apparent to those skilled in the art.

Claims (8)

1. The rectification process for separating the isopropanol-diisopropyl ether-water mixture is characterized by comprising a three-tower mode, wherein a tower T1 is a simple pre-concentration tower, a tower T2 is a reactive extraction rectification tower, a tower T3 is a common rectification tower, and the specific rectification process comprises the following steps of:
(1) After heat exchange is carried out on the mixture containing isopropyl alcohol-diisopropyl ether-water and tower bottom produced materials of the tower T1 and the tower T3, the mixture enters the tower T1 from the middle part of the tower T1, the mixture is pre-concentrated, diisopropyl ether, isopropyl alcohol and water are produced from the tower top, the mixture enters the tower T2, and high-purity water is produced from the tower bottom;
(2) Ethylene oxide enters a tower T2 from the middle part of the tower T2, reacts and separates with components from the tower T1 and the tower T3 in the tower T2, high-purity diisopropyl ether is extracted from the tower top, isopropanol, ethylene glycol, trace water and ethylene oxide are extracted from the tower bottom, and the mixture enters the tower T3;
(3) The components from the tower T2 are separated in a tower T3, high-purity isopropanol is separated from the tower top, high-purity ethylene glycol is extracted from the tower bottom, part of the high-purity ethylene glycol is cooled and then enters the tower T2 for circulation, and the rest of the high-purity ethylene glycol is extracted.
2. The rectification process for separating an isopropyl alcohol-diisopropyl ether-water mixture according to claim 1, wherein the operation pressure of the column T1 is 101kPa, the column top temperature is 60 to 63 ℃, the column bottom temperature is 102 to 106 ℃, the theoretical plate number is 14 to 20, the reflux ratio is 0.7 to 0.8, and the mixture feed position of isopropyl alcohol-diisopropyl ether-water is 10 to 13 th plate.
3. The rectification process for separating an isopropyl alcohol-diisopropyl ether-water mixture according to claim 2, wherein the column T2 has an operating pressure of 101kPa, a column top temperature of 66 to 70 ℃, a column bottom temperature of 115 to 125 ℃, a theoretical plate number of 25 to 37 plates, a reflux ratio of 1.3 to 1.7, a feeding position of the component from the column T1 of 5 to 7 plates, a feeding position of the component from the column T3 of 2 to 4 plates, and a feeding position of the ethylene oxide of 12 to 14 plates.
4. A rectification process for separating an isopropyl alcohol-diisopropyl ether-water mixture according to claim 3, wherein the operating pressure of the column T3 is 101kPa, the column top temperature is 80-83 ℃, the column bottom temperature is 200-205 ℃, the theoretical number of plates is 21-27, the reflux ratio is 2.2-2.8, and the feeding position of the component from the column T2 is 11-15 plates.
5. The rectification process for separating an isopropyl alcohol-diisopropyl ether-water mixture according to claim 1, wherein the mass ratio of isopropyl alcohol, diisopropyl ether and water in the isopropyl alcohol-diisopropyl ether-water mixture is 1:2-4:5-7.
6. A rectification process for separating an isopropyl alcohol-diisopropyl ether-water mixture according to claim 1, characterized in that the ratio of ethylene oxide to isopropyl alcohol-diisopropyl ether-water mixture flow is between 5 and 7:100.
7. the rectification process for separating an isopropyl alcohol-diisopropyl ether-water mixture according to claim 1, wherein the purity of the high purity diisopropyl ether is 99.95-99.98%, the purity of the high purity isopropyl alcohol is 99.69-99.71%, the purity of the high purity water is 99.97-99.99%, and the purity of the high purity ethylene glycol is 99.97-99.99%.
8. A rectification process for separating an isopropyl alcohol-diisopropyl ether-water mixture according to claim 1, characterized in that the ratio of the flow of high-purity ethylene glycol to the flow of high-purity ethylene glycol extracted entering the column T2 is 4:0.6-1.
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Publication number Priority date Publication date Assignee Title
US6069284A (en) * 1998-06-17 2000-05-30 Uop Llc Process for separating diisopropyl ether from isopropyl alcohol and 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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Publication number Priority date Publication date Assignee Title
US6069284A (en) * 1998-06-17 2000-05-30 Uop Llc Process for separating diisopropyl ether from isopropyl alcohol and 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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