CN106631795B - Method for separating isopropyl acetate and n-heptane azeotrope by heat integrated pressure swing distillation - Google Patents
Method for separating isopropyl acetate and n-heptane azeotrope by heat integrated pressure swing distillation Download PDFInfo
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- C07C67/52—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation
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Abstract
The invention relates to a method for separating an isopropyl acetate and n-heptane azeotrope by heat-integrated pressure-swing distillation. Cyclohexane is used as an entrainer to separate an isopropyl acetate-n-heptane azeotrope, the isopropyl acetate and n-heptane azeotrope form the lowest azeotrope under normal pressure, the azeotropic composition is insensitive to pressure change, a third substance is added into a mixture material to form the lowest pressure sensitivity azeotrope with the isopropyl acetate in the raw material, the azeotropic point is lower than the boiling point of the isopropyl acetate-n-heptane azeotrope, a connecting line between the two azeotropic points divides a rectification area into two, low-pressure and high-pressure operation is carried out through double towers, and the separation of the mixture is realized in different rectification areas.
Description
[ technical field ] A method for producing a semiconductor device
The invention belongs to the field of chemical separation and purification, and relates to a method for separating isopropyl acetate and n-heptane azeotrope by heat-integrated pressure-swing distillation, in particular to a method for separating the lowest azeotrope with insensitive pressure by using a special entrainer.
[ background of the invention ]
Isopropyl acetate is mainly used as a solvent for paints, printing inks and the like, is also a dehydrating agent commonly used in industry, an extracting agent and a perfume component in medicine production, and is mainly used as an extracting solvent for medicines, a paint solvent, a printing ink solvent, a chemical reaction solvent and the like. The product has fruit fragrance, has apple fragrance after being diluted, is an edible spice which is allowed to be used in China GB2760-86 regulations, is mainly used for preparing rum essence and a solvent of fruit type spices, and is widely applied to the food and drug industry. N-heptane is a typical nonpolar solvent, is used as a standard substance for the determination of n-heptane value, and can be used as anesthetic, solvent and raw material for organic synthesis, and preparation of experimental reagent. It can be widely used for producing paint, dye, pigment, printing ink, adhesive, medicine, pesticide, food additive, feed additive, essence, perfume and cosmetics. Isopropyl acetate forms the lowest azeotrope under normal pressure, the azeotropic composition is insensitive to pressure change, and the isopropyl acetate cannot be completely separated by adopting a common pressure swing rectification method.
The patent (CN1090298A) discloses a method for separating and preparing aloe-emodin and rhein by using isopropyl acetate and n-heptane as solvents, wherein the separation purity of the aloe-emodin and rhein respectively reaches 98%.
the patent (CN103450331A) discloses a method for refining a pharmaceutical compound, namely bortezomib, by using isopropyl acetate and n-heptane as organic solvents, adding water into a bortezomib crude product to adjust the pH value to be alkaline for dissolution, adding an organic solvent to wash and remove water-soluble impurities, adding an organic solvent into a water layer to adjust acid, removing water-soluble impurities under an acidic condition, adding an organic solvent, a cosolvent and a decolorizing agent into an organic layer feed liquid after concentration, and crystallizing to obtain high-purity bortezomib.
the patent (CN105001056A) discloses a method for separating isobutanol and n-heptane azeotrope by pressure swing distillation and a device suitable for the method, wherein the method utilizes the isobutanol and n-heptane system to successfully separate isobutanol and n-heptane binary azeotrope and obtain two products with higher purity by the following steps of pressure rise, azeotropic composition shift and azeotropic behavior respectively show the lowest azeotropic characteristic and the highest azeotropic characteristic.
The patent (CN105001056A) discloses a method for separating an ethanol and tetrahydrofuran azeotrope by low-pressure and high-pressure double-tower rectification, which utilizes the fact that the azeotropic composition of the ethanol and tetrahydrofuran is greatly changed along with the change of pressure, firstly adopts normal-pressure rectification to process fresh materials, and then adopts a pressurized rectifying tower to rectify and purify, and ethanol and tetrahydrofuran products are respectively extracted from the bottoms of the normal-pressure tower and the high-pressure tower.
The patent (CN103055530A) discloses a method for separating cyclohexanone and phenol by solvent-enhanced pressure swing thermal coupling rectification, wherein cyclohexanone and phenol form the highest azeotrope with insensitive pressure under normal pressure, acetophenone or benzaldehyde solvent is added for separating cyclohexanone and phenol by pressure swing rectification, and the separation method has certain guiding significance for the separation of the highest azeotrope with insensitive pressure.
The invention adopts cyclohexane as entrainer to separate the azeotrope of isopropyl acetate and n-heptane by pressure swing distillation, and has obvious economic, environmental and social benefits. Isopropyl acetate and n-heptane form the lowest azeotrope under normal pressure, the azeotropic composition is insensitive to pressure change, and the isopropyl acetate and the n-heptane are difficult to be completely separated by adopting common pressure swing rectification. The third substance added in the mixture material and the isopropyl acetate in the raw material form an azeotrope with lowest pressure sensitivity, the azeotropic point is lower than the boiling point of the isopropyl acetate and the n-heptane azeotrope, the connecting line between the two azeotropic points forms a rectification boundary, the rectification area is divided into two areas, and the low-pressure and high-pressure operation is carried out through double towers, so that the separation of the mixture is realized in different rectification areas. Therefore, the separation method has certain guiding significance on the separation of the lowest azeotrope which is insensitive to the pressure.
[ summary of the invention ]
[ problem to be solved ]
The invention aims to provide a device for separating isopropyl acetate and n-heptane azeotrope based on heat integration pressure swing distillation.
It is another object of the present invention to provide a process for separating an azeotrope of isopropyl acetate and n-heptane using said apparatus.
It is another object of the invention to provide a process for separating the lowest azeotropes for which the apparatus is not sensitive to such pressures.
[ solution ]
The invention is realized by the following technical scheme.
A method for separating isopropyl acetate and n-heptane azeotrope by heat integrated pressure swing distillation is characterized in that the device used by the method mainly comprises the following parts:
A vacuum tower (T1), a reboiler (R1), a condenser (C1), a reflux tank (D1), a pressure pump (P1), a high-pressure tower (T2), a reboiler (R2), a reflux tank (D2) and a pressure pump (P2); wherein the condenser (C1), the reflux tank (D1) and the pressure pump (P1) are sequentially connected with the top of the vacuum tower (T1) through pipelines, the reboiler (R1) is connected with the bottom of the vacuum tower (T1), the reflux tank (D2) and the pressure pump (P2) are sequentially connected with the top of the high-pressure tower (T2) through pipelines, and the reboiler (R2) is connected with the bottom of the high-pressure tower (T2).
The method comprises the following steps:
(1) Conveying a raw material mixed solution of isopropyl acetate and n-heptane to the middle part of a pressure reducing tower (T1) through a pressure reducing valve, introducing cyclohexane serving as an entrainer from the top of the pressure reducing tower (T1), condensing steam at the top of the pressure reducing tower (T1) through a condenser (C1), collecting the steam in a reflux tank (D1), pressurizing the steam through a pressure pump (P1), conveying partial materials to the top of the pressure reducing tower (T1) for reflux, and conveying partial materials to a high-pressure tower (T2) for secondary rectification;
(2) The bottom material of the vacuum tower (T1) is reboiled by a reboiler (R1) and enters the vacuum tower (T1), and part of the material is extracted as a high-purity isopropyl acetate product;
(3) the steam at the top of the high-pressure tower (T2) enters a reboiler (R1) to exchange heat with the material at the bottom of the vacuum tower (T1), so that complete heat integration is realized; after heat exchange, the steam at the top of the high-pressure tower (T2) is completely condensed and conveyed to a reflux tank (D2) for collection, after being pressurized by a pressure pump (P2), part of the materials are conveyed to the top of the high-pressure tower (T2) for reflux, and part of the materials are conveyed to a pressure reduction tower (T1) for circular rectification;
(4) the bottom material of the high pressure tower (T2) is reboiled by a reboiler (R2) and enters the high pressure tower (T2), and part of the material is extracted as a high-purity n-heptane product;
According to another preferred embodiment of the invention, it is characterized in that: isopropyl acetate and n-heptane form the lowest azeotrope under normal pressure, the azeotropic composition is insensitive to pressure change, and the isopropyl acetate and the n-heptane are difficult to be completely separated by adopting common pressure swing rectification. After the entrainer is added, a rectification boundary is formed, and low-pressure and high-pressure operation is carried out through the double towers, so that the separation of the mixture is realized in different rectification areas.
According to another preferred embodiment of the invention, the entrainer added to the mixture is such that it satisfies the following conditions:
(1) the entrainer and the isopropyl acetate form a minimum azeotrope, and the isopropyl acetate, the n-heptane and the entrainer do not form a ternary azeotrope;
(2) The boiling point of the entrainer and the minimum azeotrope of the isopropyl acetate is lower than that of an azeotrope of the isopropyl acetate and the n-heptane;
(3) the entrainer forms a minimal azeotrope with isopropyl acetate, the composition of which is sensitive to pressure variations with a composition deviation of greater than 5%.
According to another preferred embodiment of the invention, it is characterized in that: the operating pressure of the decompression tower (T1) is 0.1atm absolute pressure, the theoretical plate number is 41, the position of the feed plate is 19-23, the position of the cyclohexane circulating material flow feed plate is 11-17, the reflux ratio is 0.27-2.0, the temperature of the top of the tower is 21-36 ℃, and the temperature of the bottom of the tower is 61-67 ℃; the operating pressure of the high-pressure tower (T2) is 6atm absolute pressure, the theoretical plate number is 48, the position of a feed plate is 4-6, the reflux ratio is 0.9-3.6, the temperature of the top of the tower is 147-155 ℃, and the temperature of the bottom of the tower is 176-184 ℃.
According to another preferred embodiment of the invention, it is characterized in that: the mass ratio of the added entrainer to the mixed material is 1.3-1.8.
According to another preferred embodiment of the invention, it is characterized in that: the mass fraction of isopropyl acetate in the mixed material is more than 80%.
According to another preferred embodiment of the invention, it is characterized in that: the purity of the separated isopropyl acetate is 99.86-99.92%, the recovery rate of the isopropyl acetate is 99.86-99.92%, the purity of the n-heptane is 99.90-99.96%, and the recovery rate of the n-heptane is 99.90-99.96%.
The method for separating isopropyl acetate and n-heptane by heat integration pressure swing distillation is specifically described as follows: the method comprises the following steps that a raw material mixed solution of isopropyl acetate and n-heptane is conveyed to a vacuum tower (T1) through a pressure reducing valve through a pipeline 2 for primary rectification, steam at the top of the vacuum tower (T1) is condensed through a condenser (C1), and is collected through a reflux tank (D1), part of materials are conveyed to the top of the vacuum tower (T1) through a pressure pump (P1) through a pipeline 3 for reflux, and part of materials are conveyed to a high-pressure tower (T2) through a pipeline 4 for secondary rectification; the bottom material of the vacuum tower (T1) is reboiled by a reboiler (R1) and then enters the vacuum tower (T1) through a pipeline 5, and part of the material is taken as a high-purity isopropyl acetate product and is extracted through a pipeline 6; the steam at the top of the high-pressure tower (T2) enters a reboiler (R1) through a pipeline 11 to exchange heat with the material at the bottom of the vacuum tower (T1), so that complete heat integration is realized; after heat exchange, steam at the top of the high-pressure tower (T2) is condensed and is conveyed to a reflux tank (D2) through a pipeline 12 for collection, part of materials are conveyed to the top of the high-pressure tower (T2) through a pressure pump (P2) through a pipeline 7 for reflux, and part of materials are conveyed to a pressure reducing tower (T1) through a pipeline 8 for circular rectification; the bottom material of the high pressure tower (T2) is reboiled by a reboiler (R2) and then enters the high pressure tower (T2) through a pipeline 9, and part of the material is taken as a high-purity n-heptane product and is extracted through a pipeline 10;
[ advantageous effects ]
compared with the prior art, the invention mainly has the following beneficial effects:
(1) the isopropyl acetate and the n-heptane obtained by separation have high purity.
(2) compared with the traditional pressure swing distillation, the invention has low equipment investment cost.
(3) Compared with the traditional pressure swing rectification, the invention has low energy consumption through heat integration.
[ description of the drawings ]
FIG. 1 is a schematic diagram of a pressure swing distillation apparatus for separating an azeotrope of isopropyl acetate and n-heptane wherein:
T1-vacuum column; t2-high pressure column; d1, D2-reflux drum; c1-overhead condenser; r1, R2-bottoms reboiler;
P1, P2-pressure pump; the numbers indicate the respective streams.
[ detailed description ] embodiments
example 1:
the feeding flow is 1000kg/h, and the mass composition is as follows: isopropyl acetate 90%, n-heptane 10%, temperature 25 deg.C, pressure 1atm absolute pressure, and circulation flow rate 1657 kg/h. The diameter of the decompression tower (T1) is 700mm, the theoretical plate number is 41, the 19 th plate is used for feeding, the cyclohexane circulation flow is used for feeding at the 11 th plate, the operation pressure is 0.1atm absolute pressure, the reflux ratio is 0.32, the temperature at the top of the tower is 36 ℃, and the temperature at the bottom of the tower is 67 ℃; the diameter of the high-pressure tower (T2) is 570mm, the theoretical plate number is 48, the high-pressure tower is fed into the 4 th block, the operation pressure is 6atm absolute pressure, the reflux ratio is 1.1, the temperature of the top of the tower is 155 ℃, and the temperature of the bottom of the tower is 184 ℃. The quality purity of the isopropyl acetate product obtained after separation is 99.92 percent, and the yield is 99.92 percent. The purity of the n-heptane product was 99.95% and the yield was 99.95%.
TABLE 1 comparison of energy consumption for thermal integration techniques
Example 2:
The feeding flow is 1000kg/h, and the mass composition is as follows: 90 percent of isopropyl acetate and 10 percent of n-heptane, the temperature is 25 ℃, the pressure is 1atm absolute pressure, and the circulating flow is 1470 kg/h. The diameter of a decompression tower (T1) is 820mm, the theoretical plate number is 41, the decompression tower is fed at the 21 st plate, the circulating flow is fed at the 12 th plate, the operation pressure is 0.1atm absolute pressure, the reflux ratio is 0.27, the temperature at the top of the tower is 36 ℃, and the temperature at the bottom of the tower is 67 ℃; the diameter of a high-pressure tower (T2) is 530mm, the theoretical plate number is 48, the high-pressure tower is fed into the 6 th block, the operation pressure is 6atm absolute pressure, the reflux ratio is 0.9, the temperature of the top of the tower is 155 ℃, and the temperature of the bottom of the tower is 184 ℃. The quality purity of the isopropyl acetate product obtained after separation is 99.90 percent, and the yield is 99.90 percent. The purity of the n-heptane product was 99.94% and the yield was 99.94%.
TABLE 2 comparison of energy consumption for thermal integration techniques
Example 3:
The feeding flow is 1000kg/h, and the mass composition is as follows: 80% of isopropyl acetate and 20% of n-heptane, the temperature is 25 ℃, the pressure is 1atm absolute pressure, and the circulating flow is 2020 kg/h. The diameter of a decompression tower (T1) is 1300mm, the number of theoretical plates is 41, the material is fed in the 23 rd plate, the circulating flow is fed in the 13 th plate, the operation pressure is 0.1atm absolute pressure, the reflux ratio is 1.7, the temperature at the top of the tower is 21 ℃, and the temperature at the bottom of the tower is 60 ℃; the diameter of the high-pressure tower (T2) is 760mm, the theoretical plate number is 48, the high-pressure tower is fed into the 4 th tower, the operation pressure is 6atm absolute pressure, the reflux ratio is 3.1, the temperature of the top of the tower is 148 ℃, and the temperature of the bottom of the tower is 176 ℃. The quality purity of the isopropyl acetate product obtained after separation is 99.90 percent, and the yield is 99.90 percent. The purity of the n-heptane product was 99.9% and the yield was 99.90%.
TABLE 3 comparison of energy consumption for thermal integration techniques
Example 4:
the feeding flow is 1000kg/h, and the mass composition is as follows: 80% of isopropyl acetate and 20% of n-heptane, the temperature is 25 ℃, the pressure is 1atm absolute pressure, and the circulating flow is 1847 kg/h. The diameter of a decompression tower (T1) is 1200mm, the number of theoretical plates is 41, the material is fed in the 23 rd plate, the circulating flow is fed in the 17 th plate, the operation pressure is 0.1atm absolute pressure, the reflux ratio is 2.0, the temperature at the top of the tower is 21 ℃, and the temperature at the bottom of the tower is 61 ℃; the diameter of the high-pressure tower (T2) is 760mm, the theoretical plate number is 48, the high-pressure tower is fed into the 6 th block, the operation pressure is 6atm absolute pressure, the reflux ratio is 3.6, the temperature at the top of the tower is 147 ℃, and the temperature at the bottom of the tower is 176 ℃. The quality purity of the isopropyl acetate product obtained after separation is 99.86 percent, and the yield is 99.86 percent. The purity of the n-heptane product was 99.96%, and the yield was 99.96%.
TABLE 4 comparison of energy consumption for thermal integration techniques
The invention provides a method for separating isopropyl acetate and n-heptane azeotrope by heat integration pressure swing distillation, wherein cyclohexane is added, pure substances can be respectively extracted from the bottom of a tower by pressure swing distillation, and energy is saved by over 37% by adopting a heat integration mode.
Claims (4)
1. A method for separating isopropyl acetate and n-heptane azeotrope by heat integrated pressure swing distillation is characterized in that the device used by the method mainly comprises the following parts:
A vacuum tower (T1), a vacuum tower reboiler (R1), a condenser (C1), a vacuum tower reflux tank (D1), a vacuum tower pressure pump (P1), a high-pressure tower (T2), a high-pressure tower reboiler (R2), a high-pressure tower reflux tank (D2) and a high-pressure tower pressure pump (P2); wherein the condenser (C1), the decompression tower reflux tank (D1) and the decompression tower pressure pump (P1) are sequentially connected to the top of the decompression tower (T1) through pipelines, the decompression tower reboiler (R1) is connected to the bottom of the decompression tower (T1), the high-pressure tower reflux tank (D2) and the high-pressure tower pressure pump (P2) are sequentially connected to the top of the high-pressure tower (T2) through pipelines, and the high-pressure tower reboiler (R2) is connected to the bottom of the high-pressure tower (T2);
the method comprises the following steps:
(1) Conveying a raw material mixed solution of isopropyl acetate and n-heptane to the middle part of a vacuum tower (T1) through a pressure reducing valve, introducing an entrainer from the top of the vacuum tower (T1), condensing steam at the top of the vacuum tower (T1) through a condenser (C1), collecting steam in a vacuum tower reflux tank (D1), pressurizing by a vacuum tower pressure pump (P1), conveying partial materials to the top of the vacuum tower (T1) for reflux, and conveying partial materials to a high-pressure tower (T2) for secondary rectification;
(2) The bottom material of the vacuum tower (T1) is reboiled by a vacuum tower reboiler (R1) and then enters the vacuum tower (T1), and part of the material is extracted as a high-purity isopropyl acetate product;
(3) The steam at the top of the high-pressure tower (T2) enters a vacuum tower reboiler (R1) to exchange heat with the material at the bottom of the vacuum tower (T1), so that complete heat integration is realized; after heat exchange, the steam at the top of the high-pressure tower (T2) is completely condensed and conveyed to a high-pressure tower reflux tank (D2) for collection, after being pressurized by a high-pressure tower pressure pump (P2), part of the materials are conveyed to the top of the high-pressure tower (T2) for reflux, and part of the materials are conveyed to a vacuum tower (T1) for circular rectification;
(4) The bottom material of the high pressure tower (T2) is reboiled by a high pressure tower reboiler (R2) and then enters the high pressure tower (T2), and part of the material is extracted as a high-purity n-heptane product;
The entrainer is cyclohexane, and the mass ratio of the entrainer to the mixed material added into the decompression tower (T1) is 1.3-1.8; the operating pressure of the decompression tower (T1) is 0.1atm absolute pressure, the theoretical plate number is 41, the position of the feeding plate is 19-23, the position of the cyclohexane circulation material flow feeding plate is 11-17, and the reflux ratio is 0.27-2.0; the operating pressure of the high-pressure tower (T2) is 6atm, the absolute pressure theoretical plate number is 48, the position of the feed plate is 4-6, and the reflux ratio is 0.9-3.6.
2. The method for separating the azeotrope of isopropyl acetate and n-heptane by heat-integrated pressure swing distillation according to claim 1, wherein the azeotropic mixture of isopropyl acetate and n-heptane is obtained by the following steps: the temperature of the top of the vacuum tower (T1) is 21-36 ℃, the temperature of the bottom of the vacuum tower (T1) is 61-67 ℃, the temperature of the top of the high-pressure tower (T2) is 147-155 ℃, and the temperature of the bottom of the high-pressure tower (T2) is 176-184 ℃.
3. the method for separating the azeotrope of isopropyl acetate and n-heptane by heat-integrated pressure swing distillation according to claim 1, wherein the azeotropic mixture of isopropyl acetate and n-heptane is obtained by the following steps: the mass fraction of isopropyl acetate in the mixed material is more than 80%.
4. The method for separating the azeotrope of isopropyl acetate and n-heptane by heat-integrated pressure swing distillation according to claim 1, wherein the azeotropic mixture of isopropyl acetate and n-heptane is obtained by the following steps: the purity of the separated isopropyl acetate is 99.86-99.92%, the recovery rate of the isopropyl acetate is 99.86-99.92%, the purity of the n-heptane is 99.90-99.96%, and the recovery rate of the n-heptane is 99.90-99.96%.
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| CN115925546B (en) * | 2022-12-23 | 2023-10-17 | 南京长江江宇环保科技股份有限公司 | Method for separating isopropyl acetate and n-heptane mixture |
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| CN105061147A (en) * | 2015-07-17 | 2015-11-18 | 济南大学 | Batch distillation process for separating isopropanol-isopropyl acetate azeotrope through mixed extraction agent |
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