CN106966866B - Method for separating butanone-isopropanol-ethanol azeotrope through three-tower pressure swing distillation - Google Patents
Method for separating butanone-isopropanol-ethanol azeotrope through three-tower pressure swing distillation Download PDFInfo
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Abstract
The invention relates to a method for separating butanone-isopropanol-ethanol azeotrope by three-tower pressure swing distillation, which solves the problem of difficult separation caused by the existence of multiple groups of azeotropic and rectifying boundaries in a near-boiling point ternary system. The method utilizes the characteristics that the azeotropic composition and the azeotropic point are sensitive to pressure change and the boiling point sequence of pure substances changes under different pressures, and designs two separation sequences to separate the butanone-isopropanol-ethanol azeotrope. And the heat integration among the three towers is realized by a partial heat integration mode, so that the energy consumption is reduced to the maximum extent. Therefore, the method has the advantages of energy conservation, environmental protection, high purity of the separated product, simple process, cost saving and the like.
Description
[ technical field ] A method for producing a semiconductor device
The invention belongs to the field of chemical separation and purification, relates to a method for separating butanone-isopropanol-ethanol azeotrope by three-tower pressure swing distillation, and particularly relates to a method for changing azeotropic composition and azeotropic point condition of a system by pressure change.
[ background of the invention ]
Butanone is an excellent organic solvent and an organic synthetic raw material, and is mainly used as various resin solvents in the paint industry; isopropanol is an important chemical raw material, can be used for organic synthesis, and can also be widely used as an antifreezing additive of petroleum fuel, automobile and aviation fuel and the like; ethanol is the most widely used alcohol and is an important organic synthetic raw material and an organic solvent. Butanone, isopropanol and ethanol need to be introduced in the production process of some chemical products and biological products, and the mixture formed by the butanone, the isopropanol and the ethanol also needs to be separated and purified in the post-treatment process. In the Fischer-Tropsch synthesis reaction process, most of oxygen atoms in CO generate water, a small amount of water enters oxygen-containing organic matters such as aldol acid and the like, and short-chain oxygen-containing organic matters are easily dissolved in a water phase during oil-water separation, so that a certain amount of aldol acid oxygen-containing organic matters are contained in the Fischer-Tropsch synthesis reaction water. The Fischer-Tropsch synthesis reaction water contains oxygen-containing organic matters of aldol ketonic acid esters with different carbon numbers, the composition is complex, the difficulty in separating and recovering the organic matters in the water is very high, and the effective separation can be realized by multi-step combined treatment of various separation methods. According to the composition of oxygen-containing organic matters in the high-temperature Fischer-Tropsch synthesis reaction water, a reasonable initial separation principle method and indexes are determined, and the method plays a very important role in optimizing and saving energy of a reaction water separation process. A ternary mixture of butanone, isopropanol and ethanol belongs to a near-boiling point system, the maximum temperature difference among the components is only 4 ℃, and the butanone, the isopropanol and the ethanol form binary azeotropes respectively. Under the conditions of normal pressure and high pressure, the azeotropic point of butanone-isopropanol and the vertex of ethanol are saddle points, the vertex of butanone and isopropanol are stable points, the azeotropic point of butanone-ethanol is an unstable point, a rectification boundary curve points to the azeotropic point of butanone-isopropanol from the azeotropic point of butanone-ethanol, and pure substances are ethanol-butanone-isopropanol in sequence from low boiling point to high boiling point; under the condition of low pressure, the azeotropic point of butanone-isopropanol, the top point of ethanol and the top point of butanone are saddle points, the top point of isopropanol is a stable point node, the azeotropic point of butanone-isopropanol disappears, the rectification boundary disappears, and the pure substances are butanone-ethanol-isopropanol in the sequence from low boiling point to high boiling point. By adopting the traditional rectification separation method, a larger reflux ratio and a larger number of theoretical plates are needed, and the separation of the mixture can not meet the purity requirement of enterprises. Therefore, a special separation method is used to separate the ternary mixture. The pressure swing distillation is widely applied to related fields due to the advantages of simple process, no introduction of other solvents, strong heat integration and the like.
The patent (102992985A) discloses a method and a device for recovering butanone from a methanol-ethanol-butanone-benzene-water system by three-tower pressure swing rectification heat integration separation, wherein butanone is recovered from the methanol-ethanol-butanone-benzene-water system by a heat integration pressure swing rectification process, but the separation and purification of ethanol are not realized, and the mixed system does not contain isopropanol.
The patent (CN101244983A) discloses a method for separating and recovering organic matters in low-temperature Fischer-Tropsch synthesis reaction water, which adopts a series of rectification separation methods to effectively and orderly separate and recover methanol, ethanol, normal propyl alcohol, acetone and butanone in the Fischer-Tropsch synthesis reaction water, wherein the acetone yield is more than 87%, and the rest product yields are more than 90%.
The patent (CN105254532A) discloses a method for separating acetonitrile-methanol-benzene ternary azeotrope by three-tower pressure swing distillation, the mixture forms an azeotrope between two components under normal pressure, and efficient separation and recovery of acetonitrile-methanol-benzene under different operating pressures are realized by utilizing the pressure sensitive characteristic of azeotropic composition. The method is suitable for separating systems of acetonitrile-methanol-benzene and the like which form azeotrope pairwise, and is not suitable for separating butanone-isopropanol-ethanol azeotrope.
The invention adopts a method for separating butanone-isopropanol-ethanol azeotrope by three-tower pressure swing distillation, and has obvious economic, environmental and social benefits. By utilizing the characteristics that the azeotropic composition of a butanone-isopropanol-ethanol ternary system and the azeotropic point change along with the pressure change, the change conditions of a residual curve and a rectification boundary along with the pressure are researched. Butanone, isopropanol and ethanol form a binary minimum azeotrope under normal pressure, a connecting line between the two azeotropic points forms a rectification boundary, and a rectification area is divided into two areas. Under the condition of low pressure, the azeotropic point of butanone and isopropanol disappears, no rectification boundary is formed, and the boiling point sequence of each pure substance in the ternary system under high pressure and low pressure changes. The method is suitable for a ternary azeotropic system with the mass fraction of butanone being 0.7, the mass fraction of isopropanol being 0.1 and the mass fraction of ethanol being 0.2. Therefore, the separation method has certain guiding significance for the separation of the ternary azeotrope sensitive to the pressure.
[ summary of the invention ]
[ problem to be solved ]
The invention aims to provide a method for separating a butanone-isopropanol-ethanol ternary system by three-tower pressure swing distillation, which overcomes the defects of the prior art, develops an economical and feasible process route to realize the separation and recovery of a near-boiling point complex ternary system, realizes the high-efficiency separation and recycling of butanone, isopropanol and ethanol, and ensures that the purity of a butanone product after treatment is more than 99.9 percent and the recovery rate is more than 99.97 percent; the purity of the isopropanol product is more than 99.3 percent, and the recovery rate is more than 99.14 percent; the purity of the ethanol product is more than 99.3 percent, and the recovery rate is more than 99.37 percent.
[ solution ]
The invention is realized by the following technical scheme.
A method for separating butanone-isopropanol-ethanol azeotrope by three-tower pressure swing distillation is characterized in that the device used by the method mainly comprises the following parts:
butanone tower (T1), isopropanol tower (T2), ethanol tower (T3), condenser (C1), condenser (C2), condenser (C3), reflux tank (D1), reflux tank (D2), reflux tank (D3), reboiler (R1), reboiler (R2), reboiler (R3), booster pump (P1), and booster pump (P2); wherein the condenser (C1), the reflux tank (D1) and the pressure pump (P2) are sequentially connected with the top of a butanone tower (T1) through pipelines, the reboiler (R1) is connected with the bottom of the butanone tower (T1), the condenser (C2) and the reflux tank (D2) are sequentially connected with the top of an isopropanol tower (T2) through pipelines, the reboiler (R2) is connected with the bottom of the isopropanol tower (T2), the condenser (C3) and the reflux tank (D3) are sequentially connected with the top of an ethanol tower (T3) through pipelines, and the reboiler (R3) is connected with the bottom of the ethanol tower (T3);
according to the characteristic that the azeotropic point and the azeotropic composition of a butanone-isopropanol-ethanol ternary system change along with the pressure, the method for separating the butanone-isopropanol-ethanol azeotrope by three-tower pressure swing distillation has two separation sequences, namely a sequence I: butanone-isopropanol-ethanol, sequence two: isopropanol-butanone-ethanol.
The first separation sequence comprises the following steps:
(1) butanone-isopropanol-ethanol mixed solution is conveyed to the middle part of a butanone tower (T1) through a pressure pump (P1), high-purity butanone products are extracted from the bottom of the butanone tower (T1), steam at the top of the butanone tower is condensed through a condenser (C1), and is collected through a reflux tank (D1), partial materials are conveyed to the top of the butanone tower (T1) to be refluxed after being pressurized through the pressure pump (P2), and partial materials are conveyed to an isopropanol tower (T2) to be rectified for the second time;
(2) an isopropanol product is obtained at the bottom of an isopropanol tower (T2), steam at the top of the tower is condensed by a condenser (C2), and is collected by a reflux tank (D2), part of materials are conveyed to the top of the isopropanol tower (T2) for reflux, and part of materials are conveyed to an ethanol tower (T3) for secondary rectification;
(3) an ethanol product is obtained at the bottom of the ethanol tower (T3), steam at the top of the tower is condensed by a condenser (C3), and is collected by a reflux tank (D3), part of materials are conveyed to the top of the ethanol tower (T3) for reflux, and part of materials are conveyed to a butanone tower (T1) for circular rectification;
the separation sequence two comprises the following steps:
(1) butanone-isopropanol-ethanol mixed solution is conveyed to the middle part of an isopropanol tower (T2) through a pressure reducing valve, a high-purity isopropanol product is extracted from the bottom of the isopropanol tower (T2), steam at the top of the tower is condensed through a condenser (C2), and is collected through a reflux tank (D2), partial material is conveyed to the top of the isopropanol tower (T2) for reflux, and partial material is conveyed to a butanone tower (T1) for secondary rectification;
(2) butanone products are obtained at the bottom of the butanone tower (T1), the top steam is condensed by a condenser (C1), and collected by a reflux tank (D1), after being pressurized by a pressure pump (P2), partial materials are conveyed to the top of the butanone tower (T1) for reflux, and partial materials are conveyed to the ethanol tower (T3) for secondary rectification;
(3) an ethanol product is obtained at the bottom of the ethanol tower (T3), steam at the top of the tower is condensed by a condenser (C3), and is collected by a reflux tank (D3), part of materials are conveyed to the top of the ethanol tower (T3) for reflux, and part of materials are conveyed to a butanone tower (T1) for circular rectification;
according to another preferred embodiment of the invention, it is characterized in that: the purity of butanone products obtained by the separation sequence is more than 99.9 percent, and the recovery rate is more than 99.98 percent; the purity of the isopropanol product is more than 99.3 percent, and the recovery rate is more than 98.92 percent; the purity of the ethanol product is more than 99.1 percent, and the recovery rate is more than 99.47 percent.
According to another preferred embodiment of the invention, it is characterized in that: the purity of butanone products obtained by the separation sequence is more than 99.9 percent, and the recovery rate is more than 99.97 percent; the purity of the isopropanol product is more than 99.3 percent, and the recovery rate is more than 99.14 percent; the purity of the ethanol product is more than 99.3 percent, and the recovery rate is more than 99.37 percent.
According to another preferred embodiment of the invention, it is characterized in that: the steam at the top of the butanone tower (T1) can be used as a heat source to supply heat to the bottoms of the isopropanol tower (T2) and the ethanol tower (T3).
According to another preferred embodiment of the invention, it is characterized in that: the steam at the top of the butanone tower (T1) can be used as a heat source to supply heat to the bottom of the isopropanol tower (T2).
According to another preferred embodiment of the invention, it is characterized in that: the condensing mechanism of the overhead vapor of the butanone tower (T1) which is penetrated by the pipeline is an isopropanol tower (T2) reboiler and an ethanol tower (T3) reboiler.
According to another preferred embodiment of the invention, it is characterized in that: the condensing mechanism of the overhead vapor of the butanone tower (T1) which is penetrated by a pipeline is an isopropanol tower (T2) reboiler.
The invention relates to a method for separating butanone-isopropanol-ethanol azeotrope by three-tower pressure swing distillation, wherein a specific process of a separation sequence I is described as follows: butanone-isopropanol-ethanol mixed solution is conveyed to the middle part of a butanone tower (T1) through a pipeline 1 by a pressure pump (P1) for primary rectification, steam at the top of the butanone tower (T1) is condensed by a condenser (C1) and collected by a reflux tank (D1), partial material is conveyed to the top of the butanone tower (T1) for reflux through a pipeline 5 by a pressure pump (P2), and partial material is conveyed to an isopropanol tower (T2) for secondary rectification through a pipeline 6; the bottom material of the butanone tower (T1) is reboiled by a reboiler (R1) and then enters the butanone tower (T1) through a pipeline 11, and part of the material is taken as a high-purity butanone product and is extracted through a pipeline 2; after the steam at the top of the isopropanol tower (T2) is condensed by a condenser (C2) and collected by a reflux tank (D2), part of the materials are conveyed to the top of the isopropanol tower (T2) through a pipeline 7 for reflux, and part of the materials are conveyed to an ethanol tower (T3) through a pipeline 8 for secondary rectification; the bottom material of the isopropanol tower (T2) is reboiled by a reboiler (R2) and then enters the isopropanol tower (T2) through a pipeline 12, and part of the material is taken as a high-purity isopropanol product and is extracted through a pipeline 3; after the steam at the top of the ethanol tower (T3) is condensed by a condenser (C3) and collected by a reflux tank (D3), part of materials are conveyed to the top of the ethanol tower (T3) through a pipeline 9 for reflux, and part of materials are conveyed to a butanone tower (T1) through a pipeline 10 for cyclic rectification; the bottom material of the ethanol tower (T3) is reboiled by a reboiler (R3) and then enters the ethanol tower (T3) through a pipeline 13, and part of the material is taken as a high-purity ethanol product and is extracted through a pipeline 4;
the specific process of the separation sequence II is described as follows: butanone-isopropanol-ethanol mixed solution is conveyed to the middle part of an isopropanol tower (T2) through a pressure reducing valve through a pipeline 1 for primary rectification, steam at the top of the isopropanol tower (T2) is condensed through a condenser (C2) and collected through a reflux tank (D2), partial material is conveyed to the top of the isopropanol tower (T2) through a pipeline 5 for reflux, and partial material is conveyed to a butanone tower (T1) through a pipeline 6 for secondary rectification; the bottom material of the isopropanol tower (T2) is reboiled by a reboiler (R2) and then enters the isopropanol tower (T2) through a pipeline 11, and part of the material is taken as a high-purity isopropanol product and is extracted through a pipeline 2; after steam at the top of the butanone tower (T1) is condensed by a condenser (C1) and collected by a reflux tank (D1), part of materials are conveyed to the top of the butanone tower (T1) through a pressure pump (P2) through a pipeline 7 for reflux, and part of materials are conveyed to an ethanol tower (T3) through a pipeline 8 for secondary rectification; the bottom material of the butanone tower (T1) is reboiled by a reboiler (R1) and then enters the butanone tower (T1) through a pipeline 12, and part of the material is taken as a high-purity butanone product and is extracted through a pipeline 3; after the steam at the top of the ethanol tower (T3) is condensed by a condenser (C3) and collected by a reflux tank (D3), part of materials are conveyed to the top of the ethanol tower (T3) through a pipeline 9 for reflux, and part of materials are conveyed to a butanone tower (T1) through a pipeline 10 for cyclic rectification; the bottom material of the ethanol tower (T3) is reboiled by a reboiler (R3) and then enters the ethanol tower (T3) through a pipeline 13, and part of the material is taken as a high-purity ethanol product and is extracted through a pipeline 4;
[ advantageous effects ]
Compared with the prior art, the invention mainly has the following beneficial effects:
(1) the butanone, isopropanol and ethanol products obtained by separation have high purity.
(2) Compared with the traditional three-tower pressure swing rectification, the invention has the advantages of low energy consumption, simple process and low equipment investment cost.
(3) Compared with other processes, the method does not introduce other solvents, and ensures the product quality.
[ description of the drawings ]
FIG. 1 is a flow chart of a three-tower pressure swing distillation process for separating butanone-isopropanol-ethanol;
FIG. 2 is a flow chart of a three-tower pressure swing distillation process with an isopropanol-butanone-ethanol separation sequence;
FIG. 3 is a flow chart of a thermal integration three-tower pressure swing distillation process with a separation sequence of butanone-isopropanol-ethanol;
FIG. 4 is a flow chart of a thermal integration three-tower pressure swing distillation process with a separation sequence of isopropanol-butanone-ethanol;
[ detailed description ] embodiments
Example 1:
the feeding flow is 1000kg/h, the temperature is 40 ℃, and the mass composition is as follows: butanone 70%, isopropanol 10%, and ethanol 20%. The theoretical plate number of the butanone tower (T1) is 34, the raw material liquid is introduced from the 26 th plate, the circulating feeding position is the 12 th plate, the operation pressure is 4.0atm, the reflux ratio is 2.00, and the tower diameter is about 490 mm; the theoretical plate number of the isopropanol tower (T2) is 100, the produced liquid at the top of the butanone tower (T1) is introduced from the 44 th plate, the operating pressure is 1.0atm, the reflux ratio is 7.50, and the diameter of the tower is about 790 mm; the theoretical plate number of the ethanol tower (T3) is 30, the produced liquid at the top of the isopropanol tower (T2) is introduced from the 16 th plate, the operation pressure is 0.4atm, the reflux ratio is 2.40, and the diameter of the tower is about 530 mm. The purity of the butanone product after separation treatment is 0.999, the purity of the isopropanol product is 0.993, the purity of the ethanol product is 0.991, the recovery rate of the butanone is 99.98%, the recovery rate of the isopropanol is 98.92%, and the recovery rate of the ethanol is 99.47%.
TABLE 1 Process operating parameters
TABLE 2 feed and product Logistics Table
Example 2:
the feeding flow is 1000kg/h, the temperature is 40 ℃, and the mass composition is as follows: butanone 70%, isopropanol 10%, and ethanol 20%. The theoretical plate number of the isopropanol tower (T2) is 77, the raw material liquid is introduced from the 19 th plate, the operation pressure is 0.1atm, the reflux ratio is 1.80, and the diameter of the tower is about 960 mm; the theoretical plate number of the butanone tower (T1) is 35, the produced liquid at the top of the isopropanol tower (T2) is introduced from the 22 th plate, the circulating feeding position is the 17 th plate, the operating pressure is 5.8atm, the reflux ratio is 2.20, and the diameter of the tower is about 400 mm; the theoretical plate number of the ethanol tower is 32, the produced liquid at the top of the butanone tower (T1) is introduced from the 13 th plate, the operation pressure is 0.4atm, the reflux ratio is 2.10, and the diameter of the tower is about 350 mm. The purity of the butanone product after separation treatment is 0.999, the purity of the isopropanol product is 0.993, the purity of the ethanol product is 0.993, the recovery rate of the butanone is 99.97%, the recovery rate of the isopropanol is 99.14%, and the recovery rate of the ethanol is 99.37%.
TABLE 3 Process operating parameters
Table 4 feed and product stream table
Example 3:
as shown in FIG. 3, the heat integration technology can be implemented in the pressure swing distillation process of three towers of butanone-isopropanol-ethanol in the separation sequence, and the overhead vapor of the butanone tower (T1) is utilized to condense and release heat to provide heat for the isopropanol tower (T2) and the ethanol tower (T3) so as to achieve the purposes of saving energy, reducing consumption and reducing equipment investment. In the figure, a butanone tower (T1) is a high-pressure tower with the operating pressure of 4atm, butanone products with the purity of 99.9 wt% are extracted from the bottom of the tower, butanone-isopropanol-ethanol azeotrope is extracted from the top of the tower, and the temperature of the top of the tower is 118.08 ℃. The isopropanol tower (T2) is an atmospheric tower with the operating pressure of 1.0atm, the isopropanol product with the purity of 99.3 wt% is extracted from the bottom of the tower, the butanone-ethanol mixture containing a small amount of isopropanol impurities is arranged at the top of the tower, and the low temperature of the tower is 95 ℃. The ethanol tower (T3) is a decompression tower with the operating pressure of 0.4atm, ethanol products with the purity of 99.1 wt% are extracted from the bottom of the tower, butanone-ethanol mixture with a small amount of isopropanol impurities is extracted from the top of the tower, and the low temperature of the tower is 65.52 ℃. Under the separation condition, the temperature of the steam at the top of the butanone tower (T1) can be 23 ℃ higher than that of the bottom of the isopropanol tower (T2) and 52 ℃ higher than that of the bottom of the ethanol tower (T3), so that the steam at the top of the butanone tower (T1) can be used as a heat source to supply heat to the bottoms of the isopropanol tower (T2) and the ethanol tower (T3), and the E1 is an auxiliary reboiler of the isopropanol tower (T2).
TABLE 5 Total energy consumption of three-column process without and with heat integration technology
| Process for the preparation of a coating | Reboiler Total Heat load/kW | Total heat load/kW of condenser |
| Without using heat integration techniques | 1634.65 | 1725.31 |
| By heat integration techniques | 1244.75 | 1335.41 |
| Total energy saving rate | 23.85％ | 22.60％ |
Example 4:
as shown in FIG. 4, the heat integration technology can be implemented in the pressure swing distillation process of three towers of isopropanol-butanone-ethanol in the separation sequence, and the condensation heat release of the overhead vapor of the butanone tower (T1) is utilized to provide heat for the isopropanol tower (T2) so as to achieve the purposes of saving energy, reducing consumption and reducing equipment investment. In the figure, an isopropanol tower (T2) is a decompression tower with the operating pressure of 0.1atm, isopropanol products with the purity of 99.3 wt% are extracted from the bottom of the tower, a butanone-ethanol mixture containing a small amount of isopropanol impurities is extracted from the top of the tower, and the temperature of the bottom of the tower is 51.31 ℃. The butanone tower (T1) is a high-pressure tower with the operating pressure of 5.8atm, butanone products with the purity of 99.9 wt% are extracted from the bottom of the tower, butanone-ethanol azeotrope containing a small amount of isopropanol impurity is extracted from the top of the tower under the pressure, and the temperature of the top of the tower is 130.99 ℃. The ethanol tower (T3) is a decompression tower with the operating pressure of 0.4atm, ethanol products with the purity of 99.3 wt% are extracted from the bottom of the tower, butanone-ethanol azeotrope containing a small amount of isopropanol impurity is extracted from the top of the tower under the operating pressure, and the low temperature of the tower is 66.30 ℃. Under the separation condition, the temperature of the steam at the top of the butanone tower (T1) can be 80 ℃ higher than that of the tower bottom of the isopropanol tower (T2), so that the steam at the top of the butanone tower (T1) can be used as a heat source to supply heat to the tower bottom of the isopropanol tower (T2), and E1 is an auxiliary reboiler of the isopropanol tower (T2).
TABLE 6 Total energy consumption of three-column process without and with heat integration technology
Claims (7)
1. A method for separating butanone-isopropanol-ethanol azeotrope by three-tower pressure swing distillation is characterized in that the device used by the method mainly comprises the following parts:
butanone tower (T1), isopropanol tower (T2), ethanol tower (T3), condenser (C1), condenser (C2), condenser (C3), reflux tank (D1), reflux tank (D2), reflux tank (D3), reboiler (R1), reboiler (R2), reboiler (R3), booster pump (P1), and booster pump (P2); wherein the condenser (C1), the reflux tank (D1) and the pressure pump (P2) are sequentially connected with the top of a butanone tower (T1) through pipelines, the reboiler (R1) is connected with the bottom of the butanone tower (T1), the condenser (C2) and the reflux tank (D2) are sequentially connected with the top of an isopropanol tower (T2) through pipelines, the reboiler (R2) is connected with the bottom of the isopropanol tower (T2), the condenser (C3) and the reflux tank (D3) are sequentially connected with the top of an ethanol tower (T3) through pipelines, and the reboiler (R3) is connected with the bottom of the ethanol tower (T3);
according to the characteristic that the azeotropic point and the azeotropic composition of a butanone-isopropanol-ethanol ternary system change along with the pressure, the separated butanone-isopropanol-ethanol mixed solution comprises 0.7 mass fraction of butanone, 0.1 mass fraction of isopropanol and 0.2 mass fraction of ethanol, and the method for separating the butanone-isopropanol-ethanol azeotrope through three-tower pressure swing distillation has two separation sequences, namely sequence one: the operating pressure of the butanone tower is 0.4atm, the operating pressure of the isopropanol tower is 1atm, the operating pressure of the ethanol tower is 0.4atm, and the sequence II: the operation pressure of the isopropanol tower is 0.1atm, the operation pressure of the butanone tower is 5.8atm, and the operation pressure of the ethanol tower is 0.4 atm;
the separation sequence one is characterized in that the method comprises the following steps:
(1) butanone-isopropanol-ethanol mixed solution is conveyed to the middle part of a butanone tower (T1) through a pressure pump (P1), high-purity butanone products are extracted from the bottom of the butanone tower (T1), steam at the top of the butanone tower is condensed through a condenser (C1), and is collected through a reflux tank (D1), partial materials are conveyed to the top of the butanone tower (T1) to be refluxed after being pressurized through the pressure pump (P2), and partial materials are conveyed to an isopropanol tower (T2) to be rectified for the second time;
(2) an isopropanol product is obtained at the bottom of an isopropanol tower (T2), steam at the top of the tower is condensed by a condenser (C2), and is collected by a reflux tank (D2), part of materials are conveyed to the top of the isopropanol tower (T2) for reflux, and part of materials are conveyed to an ethanol tower (T3) for secondary rectification;
(3) an ethanol product is obtained at the bottom of the ethanol tower (T3), steam at the top of the tower is condensed by a condenser (C3), and is collected by a reflux tank (D3), part of materials are conveyed to the top of the ethanol tower (T3) for reflux, and part of materials are conveyed to a butanone tower (T1) for circular rectification;
the separation sequence two is characterized in that the method comprises the following steps:
(1) butanone-isopropanol-ethanol mixed solution is conveyed to the middle part of an isopropanol tower (T2) through a pressure reducing valve, a high-purity isopropanol product is extracted from the bottom of the isopropanol tower (T2), steam at the top of the tower is condensed through a condenser (C2), and is collected through a reflux tank (D2), partial material is conveyed to the top of the isopropanol tower (T2) for reflux, and partial material is conveyed to a butanone tower (T1) for secondary rectification;
(2) butanone products are obtained at the bottom of the butanone tower (T1), the top steam is condensed by a condenser (C1), and collected by a reflux tank (D1), after being pressurized by a pressure pump (P2), partial materials are conveyed to the top of the butanone tower (T1) for reflux, and partial materials are conveyed to the ethanol tower (T3) for secondary rectification;
(3) and (3) obtaining an ethanol product at the bottom of the ethanol tower (T3), condensing overhead steam through a condenser (C3), collecting the overhead steam through a reflux tank (D3), conveying part of materials to the top of the ethanol tower (T3) for reflux, and conveying part of materials to a butanone tower (T1) for circular rectification.
2. The method for separating butanone-isopropanol-ethanol azeotrope by three-tower pressure swing distillation, wherein the separation sequence of the butanone-isopropanol-ethanol azeotrope is as follows: the butanone product obtained by the separation sequence I has the purity of more than 99.9 percent and the recovery rate of more than 99.98 percent; the purity of the isopropanol product is more than 99.3 percent, and the recovery rate is more than 98.92 percent; the purity of the ethanol product is more than 99.1 percent, and the recovery rate is more than 99.47 percent.
3. The method for separating butanone-isopropanol-ethanol azeotrope by using three-tower pressure swing distillation, wherein the separation sequence of isopropanol-butanone-ethanol is as follows according to claim 1, and the method comprises the following steps: the purity of butanone products obtained by the separation sequence II is more than 99.9 percent, and the recovery rate is more than 99.97 percent; the purity of the isopropanol product is more than 99.3 percent, and the recovery rate is more than 99.14 percent; the purity of the ethanol product is more than 99.3 percent, and the recovery rate is more than 99.37 percent.
4. The method for separating butanone-isopropanol-ethanol azeotrope by three-tower pressure swing distillation, wherein the separation sequence of the butanone-isopropanol-ethanol azeotrope is as follows: the first separation sequence can use the steam at the top of the butanone tower (T1) as a heat source to supply heat to the bottoms of the isopropanol tower (T2) and the ethanol tower (T3).
5. The method for separating butanone-isopropanol-ethanol azeotrope by using three-tower pressure swing distillation, wherein the separation sequence of isopropanol-butanone-ethanol is as follows according to claim 3, and the method comprises the following steps: and the second separation sequence can use the steam at the top of the butanone tower (T1) as a heat source to supply heat to the bottom of the isopropanol tower (T2).
6. The method for separating butanone-isopropanol-ethanol azeotrope by three-tower pressure swing distillation, wherein the separation sequence of the butanone-isopropanol-ethanol azeotrope is as follows: the separation sequence-condensation mechanism that can be traversed by piping with the overhead vapor of the butanone column (T1) is the isopropanol column (T2) reboiler and the ethanol column (T3) reboiler.
7. The method for separating butanone-isopropanol-ethanol azeotrope by using three-tower pressure swing distillation, wherein the separation sequence of isopropanol-butanone-ethanol is as follows: the condensation mechanism for separating the second separation sequence by using the overhead vapor of the butanone tower (T1) and penetrating through a pipeline is an isopropanol tower (T2) reboiler.
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| CN113788746A (en) * | 2021-10-19 | 2021-12-14 | 青岛科技大学 | Method for separating butanone/isopropanol/n-heptane ternary azeotrope by three-tower pressure-swing rectification |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101244983A (en) * | 2008-03-14 | 2008-08-20 | 上海兖矿能源科技研发有限公司 | Process for separating and recovering organic matter in low-temperature Fischer-Tropsch synthesizing reaction |
| CN106242948A (en) * | 2016-07-21 | 2016-12-21 | 青岛科技大学 | A kind of it is thermally integrated variable-pressure rectification separation n-butyl alcohol and the method for octane azeotropic mixture |
| CN106431880A (en) * | 2016-09-12 | 2017-02-22 | 青岛科技大学 | Novel method for rectifying and separating acetone and isopropyl ether systems under variable pressures |
-
2017
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101244983A (en) * | 2008-03-14 | 2008-08-20 | 上海兖矿能源科技研发有限公司 | Process for separating and recovering organic matter in low-temperature Fischer-Tropsch synthesizing reaction |
| CN106242948A (en) * | 2016-07-21 | 2016-12-21 | 青岛科技大学 | A kind of it is thermally integrated variable-pressure rectification separation n-butyl alcohol and the method for octane azeotropic mixture |
| CN106431880A (en) * | 2016-09-12 | 2017-02-22 | 青岛科技大学 | Novel method for rectifying and separating acetone and isopropyl ether systems under variable pressures |
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