CN114797146A - Double-partition extraction rectifying tower - Google Patents
Double-partition extraction rectifying tower Download PDFInfo
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- CN114797146A CN114797146A CN202210518230.1A CN202210518230A CN114797146A CN 114797146 A CN114797146 A CN 114797146A CN 202210518230 A CN202210518230 A CN 202210518230A CN 114797146 A CN114797146 A CN 114797146A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/34—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping with one or more auxiliary substances
- B01D3/40—Extractive distillation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
- B01D3/141—Fractional distillation or use of a fractionation or rectification column where at least one distillation column contains at least one dividing wall
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
- B01D3/32—Other features of fractionating columns ; Constructional details of fractionating columns not provided for in groups B01D3/16 - B01D3/30
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D3/34—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping with one or more auxiliary substances
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Abstract
The invention provides a double-partition-plate extraction and rectification tower which comprises a tower body, wherein a first vertical partition plate and a second vertical partition plate are arranged in the tower body at intervals from left to right, an inner cavity of the tower body is sequentially divided into a first recovery tower, a second recovery tower and a third recovery tower from left to right by the first vertical partition plate and the second vertical partition plate, the first recovery tower is sequentially divided into a rectification section, a dehydration section and a stripping section from top to bottom, the second recovery tower is sequentially divided into the rectification section, the extraction section and the stripping section from top to bottom, the third recovery tower is sequentially divided into the rectification section and the stripping section from top to bottom, a first product side-draw outlet is formed in the first recovery tower, a second product side-draw outlet is formed in the second recovery tower, and a third product side-draw outlet is formed in the third recovery tower. Compared with the traditional multi-tower extraction rectification, the invention reduces the separation difficulty, reduces the energy consumption in the separation process, and can reduce the energy consumption cost by 15 to 25 percent.
Description
Technical Field
The invention relates to the field of separation of multicomponent azeotrope, in particular to a double-partition extractive distillation tower.
Background
The wastewater solution of ternary azeotropic mixed liquor is often formed in the production process of the actual chemical industry and the pharmaceutical industry, and if the wastewater solution is directly discharged, the environmental pollution and the resource waste are caused, so that the wastewater solution has a great prospect in recycling. The existing separation and purification device for ternary azeotropic mixed liquor generally comprises a plurality of extraction towers, but the extraction towers are too many, which can lead to complex connecting pipelines and complicated operation steps, not only increases the difficulty of separation and purification, but also increases the energy consumption of the separation process and reduces the energy utilization rate.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide a double-partition-plate extractive distillation tower which can replace the traditional multi-tower separation and realize the separation and purification of ternary azeotropic mixed liquid through a single tower, thereby reducing the separation difficulty and reducing the energy consumption in the separation process.
In order to achieve the purpose, the invention provides a double-partition-plate extractive distillation tower, which comprises a tower body, wherein a first vertical partition plate and a second vertical partition plate are arranged in the tower body at intervals from left to right, the inner cavity of the tower body is sequentially divided into a first recovery tower, a second recovery tower and a third recovery tower by the first vertical partition plate and the second vertical partition plate from left to right, the upper ends and the lower ends of the first vertical partition plate and the second vertical partition plate are respectively spaced from the top and the bottom of the tower body, a first transverse partition plate is arranged between the top end of the first vertical partition plate and the left side wall of the tower body, the height of the lower end of the first vertical partition plate is lower than that of the lower end of the second vertical partition plate, a third transverse partition plate is arranged between the top end of the second vertical partition plate and the right side wall of the tower body, a second transverse partition plate extending towards the second vertical partition plate is arranged at the bottom end of the first vertical partition plate, and the right end of the second transverse partition plate extends to the lower part of the second vertical partition plate and then is bent downwards to form a bent part, the tower is characterized in that a fourth transverse partition plate and a fifth transverse partition plate are respectively arranged on the left side wall and the right side wall of the tower body, the fourth transverse partition plate and the fifth transverse partition plate are respectively positioned on the left side and the right side of the lower end of the bent portion and form a first channel and a second channel with the bent portion, a sixth transverse partition plate is arranged above the fifth transverse partition plate, the right end of the sixth transverse partition plate is fixed on the right side wall of the tower body, the left end of the sixth transverse partition plate extends to the lower side of the second vertical partition plate and forms a third channel with the lower side of the second vertical partition plate, a fourth channel is formed between the left end of the sixth transverse partition plate and the second transverse partition plate, the fourth transverse partition plate is positioned between the gas stripping section and the dewatering section of the first recovery tower, the first recovery tower is sequentially divided into the gas stripping section, the dewatering section and the gas stripping section from top to bottom, and the second recovery tower is sequentially divided into the rectifying section from top to bottom, The third recovery tower is internally divided into a rectifying section and a stripping section from top to bottom in sequence;
a second mixed liquid side line extraction outlet is arranged at the top of the first recovery tower, a first mixed liquid inlet is arranged at the upper part of the first recovery tower, a first product side line extraction outlet is arranged at the middle part of the first recovery tower, a tower bottom liquid extraction outlet is arranged at the bottom of the first recovery tower, a second product extraction outlet is arranged at the top of the second recovery tower, an extraction solvent side line inlet is arranged at the upper part of the second recovery tower, a second mixed liquid side line inlet is arranged at the middle part of the second recovery tower, and a third product side line extraction outlet is arranged at the top of the third recovery tower.
In the scheme, the method comprises the following steps: the extraction outlet of the first product side line is provided with a first product extraction line, the extraction outlet of the tower kettle liquid extraction port is connected with a reboiler, the bottom of the first recovery tower is also provided with a tower kettle liquid return port, the reboiler is provided with a return pipe connected with the tower kettle liquid return port, the reboiler is also provided with an extraction line connected with an extraction solvent condenser, and the extraction solvent condenser is connected with an extraction solvent side line inlet through the extraction line.
In the scheme, the method comprises the following steps: an extraction solvent supplement line is also arranged on a withdrawal line between the extraction solvent condenser and the extraction solvent side line inlet.
In the scheme, the method comprises the following steps: a withdrawal line is arranged at a side withdrawal port of the second mixed liquid and connected with a second mixed liquid condenser, the second mixed liquid condenser is connected with a second mixed liquid return tank, a return port is further arranged at the top of the first recovery tower, a return pipe is arranged on the second mixed liquid return tank and connected with the return port, and a withdrawal line is further arranged on the second mixed liquid return tank and connected with a side inlet of the second mixed liquid.
In the scheme, the method comprises the following steps: the extraction line is arranged at the extraction outlet of the second product and is connected with a second product condenser, the second product condenser is connected with a second product reflux tank, a second product reflux port is further arranged at the top of the extraction rectification tower, a reflux pipe is arranged on the second product reflux tank and is connected with the second product reflux port, and a second product extraction line is further arranged on the second product reflux tank.
In the scheme, the method comprises the following steps: an extraction line is arranged at a third product side line extraction port and connected with a third product condenser, the third product condenser is connected with a third product reflux tank, a third product reflux port is further arranged at the top of the third product recovery tower, a reflux pipe is arranged on the third product reflux tank and connected with the third product reflux port, and a third product extraction line is further arranged on the third product reflux tank.
In the scheme, the method comprises the following steps: the number of theoretical plates of the first recovery tower is 38-42, the first mixed liquid inlet is positioned at 8-12 plates, the first product side draw outlet is positioned at 23-27 plates, the first channel is positioned at 30-34 plates, the rectifying section is positioned between 1-10 plates, the dehydrating section is positioned between 10-32 plates, and the stripping section is positioned between 32-40 plates.
In the scheme, the method comprises the following steps: the theoretical plate number of the second recovery tower is 38-42, the side inlet of the extraction solvent is positioned at 3-5 plates, the side inlet of the second mixed liquid is positioned at 23-27 plates, and the fourth channel is positioned at the bottommost part of the second recovery tower.
In the scheme, the method comprises the following steps: the theoretical plate number of the third recovery tower is 38-42, the third channel is positioned at 23-27 plates, and the fourth channel is positioned at the bottommost part of the methanol recovery tower.
The invention has the beneficial effects that:
1. the inner cavity of the single tower is divided into three independent subareas by the two vertical clapboards and the plurality of transverse clapboards, compared with the traditional multi-tower extraction rectification, the separation difficulty is reduced, the energy consumption in the separation process is reduced, and the energy consumption cost can be reduced by 15 to 25 percent.
2. Compared with the multi-tower extractive distillation, the single-tower extractive distillation has the advantages of less equipment, simpler operation, enhanced practicability and contribution to industrial popularization and use.
Drawings
Fig. 1 is a schematic structural view of a tower body.
FIG. 2 is a flow chart of a process according to the present invention.
Detailed Description
Example 1
As shown in fig. 1-2, a method for separating and purifying an ethyl acetate-methanol-water ternary azeotropic mixture, which uses dimethyl sulfoxide as an extraction solvent, uses a double-partition extractive distillation tower as a separation and purification device, and comprises a tower body.
A first vertical clapboard a and a second vertical clapboard b are arranged in the tower body at intervals from left to right, the inner cavity of the tower body is sequentially divided into a first recovery tower 1, a second recovery tower 2 and a third recovery tower 3 by the first vertical clapboard a and the second vertical clapboard b from left to right, the upper and lower ends of the first vertical clapboard a and the second vertical clapboard b are respectively spaced from the top and the bottom of the tower body, a first transverse clapboard c is arranged between the top end of the first vertical clapboard a and the left side wall of the tower body, the lower end of the first vertical clapboard a is lower than the lower end of the second vertical clapboard b, a third transverse clapboard e is arranged between the top end of the second vertical clapboard b and the right side wall of the tower body, a second transverse clapboard d extending towards the second vertical clapboard b is arranged at the bottom end of the first vertical clapboard a, and the right end of the second transverse clapboard d is bent downwards after extending to the lower part of the second vertical clapboard b to form a bending part, a fourth transverse clapboard f and a fifth transverse clapboard g are respectively arranged on the left side wall and the right side wall of the tower body, the fourth transverse clapboard f and the fifth transverse clapboard g are respectively positioned at the left side and the right side of the lower end of the bending part, a first channel A and a second channel B are respectively formed between the fourth transverse clapboard f and the bending part, a sixth transverse clapboard j is arranged above the fifth transverse clapboard g, the right end of the sixth transverse clapboard j is fixed on the right side wall of the tower body, the left end of the sixth transverse clapboard j extends to the lower part of the second vertical clapboard B, a third channel C is formed between the left end of the sixth transverse clapboard j and the lower part of the second vertical clapboard B, a fourth channel D is formed between the left end of the sixth transverse clapboard j and the second transverse clapboard D, the fourth transverse clapboard f is positioned between a gas stripping section and a dehydration section in the first recovery tower 1, the first recovery tower 1 is sequentially divided into a rectifying section, a dehydration section and a stripping section from top to bottom, and the second recovery tower 2 is sequentially divided into a rectifying section, a dehydration section and a dehydration section, An extraction section and a stripping section, wherein the third recovery tower 3 is internally divided into a rectification section and a stripping section from top to bottom in sequence;
a second mixed liquor side draw outlet 102 is arranged at the top of the first recovery tower 1, a first mixed liquor inlet 101 is arranged at the upper part, a first product side draw outlet 103 is arranged at the middle part, a tower bottom draw outlet 104 is arranged at the bottom, a second product draw outlet 105 is arranged at the top of the second recovery tower 2, an extraction solvent side draw inlet 106 is arranged at the upper part, a second mixed liquor side draw inlet 107 is arranged at the middle part, and a third product side draw outlet 108 is arranged at the top of the third recovery tower 3.
A withdrawal line is arranged at the tower bottom withdrawal port 104 and connected with the reboiler 11, a tower bottom reflux port is further arranged at the bottom of the first recovery tower 1, a reflux pipe is arranged on the reboiler 11 and connected with the tower bottom reflux port, a withdrawal line is further arranged on the reboiler 11 and connected with the extraction solvent condenser 12, and the extraction solvent condenser 12 is connected with the extraction solvent side inlet 106 through the withdrawal line.
An extraction solvent addition line 109 is also provided on the withdrawal line between the extraction solvent condenser 12 and the extraction solvent side inlet 106.
A withdrawal line is arranged at the withdrawal outlet 102 of the lateral line of the second mixed liquid and is connected with a condenser 4 of the second mixed liquid, the condenser 4 of the second mixed liquid is connected with a reflux tank 5 of the second mixed liquid, a reflux port is also arranged at the top of the first recovery tower 1, a reflux pipe is arranged on the reflux tank 5 of the second mixed liquid and is connected with the reflux port, and the withdrawal line is also arranged on the reflux tank 5 of the second mixed liquid and is connected with a lateral line inlet 107 of the second mixed liquid.
An extraction line is arranged at the second product extraction outlet 105 and connected with a second product condenser 7, the second product condenser 7 is connected with a second product reflux tank 8, a second product reflux port is further arranged at the top of the extraction rectifying tower 2, a reflux pipe is arranged on the second product reflux tank 8 and connected with the second product reflux port, and a second product extraction line is further arranged on the second product reflux tank 8.
A collecting line is arranged at a third product side line collecting outlet 108 and is connected with a third product condenser 9, the third product condenser 9 is connected with a third product reflux tank 10, a third product reflux opening is also arranged at the top of the third product recovery tower 3, a reflux pipe is arranged on the third product reflux tank 10 and is connected with the third product reflux opening, and a third product collecting line is also arranged on the third product reflux tank 10.
The theoretical plate number of the first recovery tower 1 is 38-42, the first mixed liquid inlet 101 is positioned at 8-12 plates, the first product side draw outlet 103 is positioned at 23-27 plates, the first passage A is positioned at 30-34 plates, the rectifying section is positioned between 1-10 plates, the dehydrating section is positioned between 10-32 plates, and the stripping section is positioned between 32-40 plates.
The theoretical plate number of the second recovery column 2 is 38-42, the extraction solvent side inlet 106 is located at 3-5 plates, the second mixed liquor side inlet 107 is located at 23-27 plates, and the fourth passage D is located at the bottommost part of the second recovery column 2.
The theoretical plate number of the third recovery column 3 is 38-42, the third channel C is located at 23-27 plates, and the fourth channel B is located at the bottommost part of the methanol recovery column 3.
When the double-partition-plate extractive distillation tower is applied to ethyl acetate-methanol-water separation, the first recovery tower 1 is a dehydration and solvent recovery tower, the second recovery tower 2 is an extractive distillation tower, the third recovery tower 3 is a methanol recovery tower, the first channel A is a water-dimethyl sulfoxide gas inlet and outlet, the second channel B is a first water-dimethyl sulfoxide mixed gas inlet, the third channel C is a methanol-dimethyl sulfoxide mixed gas outlet and mixed gas inlet C, and the fourth channel D is a second water-dimethyl sulfoxide mixed gas inlet D. The second mixed liquor side draw outlet 102 is an ethyl acetate-methanol side draw outlet, the first mixed liquor inlet 101 is an ethyl acetate-methanol-water mixed liquor inlet, the first product side draw outlet 103 is a water side draw outlet, the second product side draw outlet 105 is an ethyl acetate side draw outlet, the second mixed liquor side draw inlet 107 is an ethyl acetate-methanol side draw inlet, and the third product side draw outlet 108 is a methanol side draw outlet. The second mixed liquid condenser 4 is an ethyl acetate-methanol condenser, the second mixed liquid reflux tank 5 is an ethyl acetate-methanol reflux tank, the second product condenser 7 is an ethyl acetate condenser, the second product reflux tank 8 is an ethyl acetate reflux tank, the third product condenser 9 is a methanol condenser, the third product reflux tank 10 is a methanol reflux tank, and the extraction solvent condenser 12 is a dimethyl sulfoxide condenser.
Adding the ethyl acetate-methanol-water mixed solution into a dehydration and solvent recovery tower from an ethyl acetate-methanol-water mixed solution inlet, extracting water from a water side line extraction outlet in the middle of the dehydration and solvent recovery tower, condensing the water by a water condenser 6 to realize water separation, introducing water-dimethyl sulfoxide mixed gas at the bottom of the tower into the upper layer of the dehydration and solvent recovery tower through a water-dimethyl sulfoxide gas inlet and an extraction outlet, and simultaneously introducing the water-dimethyl sulfoxide mixed gas at the bottom of the tower into an extractive distillation tower and a methanol recovery tower through a first water-dimethyl sulfoxide mixed gas inlet respectively.
The tower bottom liquid of the dehydration and solvent recovery tower is extracted through a tower bottom liquid extraction outlet 104, heated by a reboiler 11 and partially refluxed to the tower bottom of the tower body, and the other part is condensed by a dimethyl sulfoxide condenser and mixed with the additional extraction solvent, and then enters from an extraction solvent side inlet 106. And after being extracted from an ethyl acetate-methanol side extraction outlet, the ethyl acetate-methanol mixed solution flows into an ethyl acetate-methanol reflux tank after being condensed by an ethyl acetate-methanol condenser, then one part of the ethyl acetate-methanol mixed solution flows back to the top of the dehydration and solvent recovery tower, and the other part of the ethyl acetate-methanol mixed solution enters the extraction rectification tower through an ethyl acetate-methanol side extraction inlet. And the ethyl acetate is extracted from an ethyl acetate extraction outlet, condensed by an ethyl acetate condenser and then flows into an ethyl acetate reflux tank, then one part of the ethyl acetate refluxes to the top of the extraction rectifying tower, and the other part of the ethyl acetate is extracted as an ethyl acetate product. The methanol is extracted from a methanol side line extraction port at the top of the methanol recovery tower, condensed by a methanol condenser and then flows into a methanol reflux tank, and then one part of the methanol is refluxed to the top of the methanol recovery tower, and the other part of the methanol is extracted as a methanol product.
The feeding molar ratio of the dimethyl sulfoxide to the mixed solution of the ethyl acetate, the methanol and the water is 0.6 to 0.7, and the feeding temperature of the mixed solution of the ethyl acetate, the methanol and the water is 35 to 45 ℃.
The temperature of the top of the dehydration and solvent recovery tower is 63-64 ℃, the temperature of the bottom of the dehydration and solvent recovery tower is 197-.
The mol reflux ratio of the extraction and rectification tower is 2.5-3.5, the dosage of the dimethyl sulfoxide is 60-70kmol/h, the feeding temperature of the dimethyl sulfoxide is 35-45 ℃, the temperature of the top of the tower is 76-77 ℃, the temperature of the bottom of the tower is 107-108 ℃, and the operating pressure is 1.0bar (absolute pressure).
The molar reflux ratio of the methanol recovery tower is 2.0-2.8, the flow rate of the methanol-dimethyl sulfoxide mixed gas extracted from the methanol-dimethyl sulfoxide mixed liquid outlet and the mixed gas inlet is 30-40kmol/h, the temperature at the top of the tower is 64-65 ℃, the temperature at the bottom of the tower is 174-175 ℃, and the operating pressure is 1.0bar (absolute pressure).
Application example 1
The mixed solution of a certain chemical pharmaceutical enterprise is separated and then comprises the following components: 5% ethyl acetate, 5% methanol, and 90% water.
The operating parameters of the dehydration and solvent recovery column were: the operating pressure is 1.0bar (absolute pressure), the number of theoretical plates is 40, the inlet of the ethyl acetate-methanol-water mixed liquid is positioned at a block tower plate, the water side line extraction outlet is positioned at a 25-block tower plate, the water-dimethyl sulfoxide gas inlet and extraction outlet are positioned at a 32-block tower plate, the temperature at the top of the tower is 63.85 ℃, the temperature at the bottom of the tower is 197.5 ℃, the rectifying section is positioned between the 1 st and 10 th tower plates, the dehydrating section is positioned between the 10 th and 32 th tower plates, and the stripping section is positioned between the 32 th and 40 th tower plates. The feeding amount of the ethyl acetate-methanol-water mixed solution is 100kmol/h, the molar reflux ratio of the dehydration and solvent recovery tower is 2.4, and the flow rate of the produced water-dimethyl sulfoxide mixed gas at the water-dimethyl sulfoxide gas inlet and the production outlet is 55 kmol/h.
Water is extracted from a water side line extraction port in the middle of the dehydration and solvent recovery tower, tower bottom liquid of the dehydration and solvent recovery tower is extracted from a tower bottom liquid extraction port, heated by a reboiler, and then partially flows back to the bottom of the tower body, and the other part is condensed by a dimethyl sulfoxide condenser, mixed with a supplemented extraction solvent, and then enters from an extraction solvent side line inlet.
And after being extracted from an ethyl acetate-methanol side extraction outlet, the ethyl acetate-methanol mixed solution flows into an ethyl acetate-methanol reflux tank after being condensed by an ethyl acetate-methanol condenser, then one part of the ethyl acetate-methanol mixed solution flows back to the top of the dehydration and solvent recovery tower, and the other part of the ethyl acetate-methanol mixed solution enters the middle part of the extractive distillation tower through an ethyl acetate-methanol side extraction inlet.
The operational parameters of the extraction and rectification tower are as follows: the operating pressure is 1.0bar (absolute pressure), the theoretical plate number is 40, the side inlet of the extraction solvent is positioned at 3 plates, the side inlet of the ethyl acetate-methanol is positioned at 25 plates, and the inlet of the second water-dimethyl sulfoxide mixed gas is positioned at the bottommost part of the extraction rectifying tower. The mol reflux ratio of the extraction and rectification tower is 2.84, the dosage of the extraction solvent dimethyl sulfoxide is 66kmol/h, the feeding temperature of the extraction solvent dimethyl sulfoxide is 40 ℃, the temperature of the top of the tower is 76.85 ℃, and the temperature of the bottom of the tower is 107.5 ℃.
And the ethyl acetate is extracted from an ethyl acetate extraction outlet, condensed by an ethyl acetate condenser and then flows into an ethyl acetate reflux tank, and then one part of the ethyl acetate flows back to the top of the extraction rectifying tower, and the other part of the ethyl acetate is extracted as an ethyl acetate product.
Operating parameters of the methanol recovery column: the operation pressure is 1.0bar (absolute pressure), the theoretical plate number is 40, the methanol-dimethyl sulfoxide mixed liquid outlet and the mixed gas inlet are positioned at 25 plates, and the first water-dimethyl sulfoxide mixed gas inlet between the steam stripping section of the dehydration and solvent recovery tower and the methanol recovery tower is positioned at the bottommost part of the methanol recovery tower. The molar reflux ratio of the methanol recovery tower is 2.39, the flow rate of the methanol-dimethyl sulfoxide mixed gas extracted from the methanol-dimethyl sulfoxide mixed liquid outlet and the mixed gas inlet is 36kmol/h, the temperature of the top of the tower is 64.15 ℃, and the temperature of the bottom of the tower is 174.5 ℃.
The methanol is extracted from a methanol side line extraction port at the top of the methanol recovery tower, condensed by a methanol condenser and then flows into a methanol reflux tank, and then one part of the methanol is refluxed to the top of the methanol recovery tower, and the other part of the methanol is extracted as a methanol product.
The purity of the separated ethyl acetate product is more than 99.5%, the purity of the separated methanol product is more than 99.5%, and the purity of the circulating extraction solvent is more than 99.99%.
Application example 2
The mixed solution of a certain chemical pharmaceutical enterprise is separated and then comprises the following components: 4.5% ethyl acetate, 4.5% methanol, and 91% water.
The operating parameters of the dehydration and solvent recovery column were: the operating pressure is 1.0bar (absolute pressure), the number of theoretical plates is 38, the inlet of the ethyl acetate-methanol-water mixed liquid is positioned at 8 plates, the water side line extraction outlet is positioned at 23 plates, the water-dimethyl sulfoxide gas inlet and extraction outlet are positioned at 30 plates, the temperature at the top of the tower is 63 ℃, the temperature at the bottom of the tower is 197 ℃, the rectifying section is positioned between the 1 st to 8 th plates, the dehydrating section is positioned between the 8 th to 30 th plates, and the stripping section is positioned between the 30 th to 38 th plates. The feeding amount of the ethyl acetate-methanol-water mixed solution is 90kmol/h, the molar reflux ratio of the dehydration and the solvent recovery tower is 2.0, and the flow rate of the produced water-dimethyl sulfoxide mixed gas at the water-dimethyl sulfoxide gas inlet and the production outlet is 50 kmol/h.
Water is extracted from a water side line extraction port in the middle of the dehydration and solvent recovery tower, tower bottom liquid of the dehydration and solvent recovery tower is extracted from a tower bottom liquid extraction port, heated by a reboiler, and then partially flows back to the bottom of the tower body, and the other part is condensed by a dimethyl sulfoxide condenser, mixed with a supplemented extraction solvent, and then enters from an extraction solvent side line inlet.
And after being extracted from an ethyl acetate-methanol side extraction outlet, the ethyl acetate-methanol mixed solution flows into an ethyl acetate-methanol reflux tank after being condensed by an ethyl acetate-methanol condenser, then one part of the ethyl acetate-methanol mixed solution flows back to the top of the dehydration and solvent recovery tower, and the other part of the ethyl acetate-methanol mixed solution enters the middle part of the extractive distillation tower through an ethyl acetate-methanol side extraction inlet.
The operational parameters of the extraction and rectification tower are as follows: the operating pressure is 1.0bar (absolute pressure), the theoretical plate number is 38, the side inlet of the extraction solvent is positioned at 4 plates, the side inlet of the ethyl acetate-methanol is positioned at 23 plates, and the inlet of the second water-dimethyl sulfoxide mixed gas is positioned at the bottommost part of the extraction rectifying tower. The mol reflux ratio of the extraction and rectification tower is 2.5, the dosage of the extraction solvent dimethyl sulfoxide is 60kmol/h, the feeding temperature of the extraction solvent dimethyl sulfoxide is 35 ℃, the temperature of the top of the tower is 76 ℃, and the temperature of the bottom of the tower is 107 ℃.
And the ethyl acetate is extracted from an ethyl acetate extraction outlet, condensed by an ethyl acetate condenser and then flows into an ethyl acetate reflux tank, and then one part of the ethyl acetate flows back to the top of the extraction rectifying tower, and the other part of the ethyl acetate is extracted as an ethyl acetate product.
Operating parameters of the methanol recovery column: the operation pressure is 1.0bar (absolute pressure), the theoretical plate number is 42, the methanol-dimethyl sulfoxide mixed liquid outlet and the mixed gas inlet are positioned at 27 plates, and the first water-dimethyl sulfoxide mixed gas inlet between the stripping section of the dehydration and solvent recovery tower and the methanol recovery tower is positioned at the bottommost part of the methanol recovery tower. The molar reflux ratio of the methanol recovery tower is 2.0, the flow of the methanol-dimethyl sulfoxide mixed gas extracted from the methanol-dimethyl sulfoxide mixed liquid outlet and the mixed gas inlet is 30kmol/h, the temperature at the top of the tower is 64 ℃, and the temperature at the bottom of the tower is 174 ℃.
The methanol is extracted from a methanol side line extraction port at the top of the methanol recovery tower, condensed by a methanol condenser and then flows into a methanol reflux tank, and then one part of the methanol is refluxed to the top of the methanol recovery tower, and the other part of the methanol is extracted as a methanol product.
The purity of the separated ethyl acetate product is more than 99.5%, the purity of the methanol product is more than 99.5%, and the purity of the circulating extraction solvent is more than 99.99%.
Application example 3
The mixed solution of a certain chemical pharmaceutical enterprise is separated and then comprises the following components: 5.5% ethyl acetate, 5.5% methanol, and 89% water.
The operating parameters of the dehydration and solvent recovery column were: the operating pressure is 1.0bar (absolute pressure), the theoretical plate number is 42, the ethyl acetate-methanol-water mixed liquid inlet is positioned at 12 plates, the water side line extraction outlet is positioned at 27 plates, the water-dimethyl sulfoxide gas inlet and extraction outlet are positioned at 34 plates, the tower top temperature is 64 ℃, the tower bottom temperature is 198 ℃, the rectifying section is positioned between the 1 st to 12 th plates, the dehydrating section is positioned between the 12 th to 34 th plates, and the stripping section is positioned between the 34 th to 42 th plates. The feeding amount of the ethyl acetate-methanol-water mixed solution is 110kmol/h, the molar reflux ratio of the dehydration and solvent recovery tower is 2.8, and the flow rate of the produced water-dimethyl sulfoxide mixed gas at the water-dimethyl sulfoxide gas inlet and the production outlet is 60 kmol/h.
Water is extracted from a water side line extraction port in the middle of the dehydration and solvent recovery tower, tower bottom liquid of the dehydration and solvent recovery tower is extracted from a tower bottom liquid extraction port, heated by a reboiler, and then partially flows back to the bottom of the tower body, and the other part is condensed by a dimethyl sulfoxide condenser, mixed with a supplemented extraction solvent, and then enters from an extraction solvent side line inlet.
And after being extracted from an ethyl acetate-methanol side extraction outlet, the ethyl acetate-methanol mixed solution flows into an ethyl acetate-methanol reflux tank after being condensed by an ethyl acetate-methanol condenser, then one part of the ethyl acetate-methanol mixed solution flows back to the top of the dehydration and solvent recovery tower, and the other part of the ethyl acetate-methanol mixed solution enters the middle part of the extractive distillation tower through an ethyl acetate-methanol side extraction inlet.
The operational parameters of the extraction and rectification tower are as follows: the operating pressure is 1.0bar (absolute pressure), the theoretical plate number is 42, the side inlet of the extraction solvent is positioned at 5 plates, the side inlet of the ethyl acetate-methanol is positioned at 27 plates, and the inlet of the second water-dimethyl sulfoxide mixed gas is positioned at the bottommost part of the extraction rectifying tower. The mol reflux ratio of the extraction and rectification tower is 3.5, the dosage of the extraction solvent dimethyl sulfoxide is 70kmol/h, the feeding temperature of the extraction solvent dimethyl sulfoxide is 45 ℃, the temperature of the top of the tower is 77 ℃, and the temperature of the bottom of the tower is 108 ℃.
And the ethyl acetate is extracted from an ethyl acetate extraction outlet, condensed by an ethyl acetate condenser and then flows into an ethyl acetate reflux tank, and then one part of the ethyl acetate flows back to the top of the extraction rectifying tower, and the other part of the ethyl acetate is extracted as an ethyl acetate product.
Operating parameters of the methanol recovery column: the operation pressure is 1.0bar (absolute pressure), the theoretical plate number is 38, the outlet of the methanol-dimethyl sulfoxide mixed liquid and the inlet of the mixed gas are positioned at 23 plates, and the inlet of the first water-dimethyl sulfoxide mixed gas between the stripping section of the dehydration and solvent recovery tower and the methanol recovery tower is positioned at the bottommost part of the methanol recovery tower. The molar reflux ratio of the methanol recovery tower is 2.8, the flow of the methanol-dimethyl sulfoxide mixed gas extracted from the methanol-dimethyl sulfoxide mixed liquid outlet and the mixed gas inlet is 40kmol/h, the temperature at the top of the tower is 65 ℃, and the temperature at the bottom of the tower is 175 ℃.
The methanol is extracted from a methanol side line extraction port at the top of the methanol recovery tower, condensed by a methanol condenser and then flows into a methanol reflux tank, and then one part of the methanol is refluxed to the top of the methanol recovery tower, and the other part of the methanol is extracted as a methanol product.
The purity of the separated ethyl acetate product is more than 99.5%, the purity of the methanol product is more than 99.5%, and the purity of the circulating extraction solvent is more than 99.99%.
Claims (9)
1. The utility model provides a two baffle extraction rectifying column, includes the tower body, its characterized in that: a first vertical clapboard (a) and a second vertical clapboard (b) are arranged in the tower body at intervals from left to right, the inner cavity of the tower body is sequentially divided into a first recovery tower (1), a second recovery tower (2) and a third recovery tower (3) from left to right by the first vertical clapboard (a) and the second vertical clapboard (b), the upper end and the lower end of the first vertical clapboard (a) and the second vertical clapboard (b) are respectively distant from the top and the bottom of the tower body, a first transverse clapboard (c) is arranged between the top end of the first vertical clapboard (a) and the left side wall of the tower body, the lower end of the first vertical clapboard (a) is lower than the lower end of the second vertical clapboard (b), a third transverse clapboard (e) is arranged between the top end of the second vertical clapboard (b) and the right side wall of the tower body, a second transverse clapboard (d) extending towards the second vertical clapboard (b) is arranged at the bottom end of the first vertical clapboard (a), the right end of the second transverse partition plate (D) extends to the lower part of the second vertical partition plate (B) and then is bent downwards to form a bent part, a left side wall and a right side wall of the tower body are respectively provided with a fourth transverse partition plate (f) and a fifth transverse partition plate (g), the fourth transverse partition plate (f) and the fifth transverse partition plate (g) are respectively positioned at the left side and the right side of the lower end of the bent part and form a first channel (A) and a second channel (B) with the bent part, a sixth transverse partition plate (j) is arranged above the fifth transverse partition plate (g), the right end of the sixth transverse partition plate (j) is fixed on the right side wall of the tower body, the left end extends to the lower part of the second vertical partition plate (B) and forms a third channel (C) with the lower part of the second vertical partition plate (B), and a fourth channel (D) is formed between the left end of the sixth transverse partition plate (j) and the second transverse partition plate (D), the fourth transverse partition plate (f) is positioned between the gas stripping section and the dehydration section in the first recovery tower (1), the first recovery tower (1) is sequentially divided into a rectification section, a dehydration section and a stripping section from top to bottom, the second recovery tower (2) is sequentially divided into a rectification section, an extraction section and a stripping section from top to bottom, and the third recovery tower (3) is sequentially divided into a rectification section and a stripping section from top to bottom;
the system is characterized in that a second mixed liquor side draw outlet (102) is arranged at the top of the first recovery tower (1), a first mixed liquor inlet (101) is arranged at the upper part, a first product side draw outlet (103) is arranged at the middle part, a tower bottom draw outlet (104) is arranged at the bottom, a second product draw outlet (105) is arranged at the top of the second recovery tower (2), an extraction solvent side draw inlet (106) is arranged at the upper part, a second mixed liquor side draw inlet (107) is arranged at the middle part, and a third product side draw outlet (108) is arranged at the top of the third recovery tower (3).
2. The double-partition extractive distillation column of claim 1, wherein: a withdrawal line is arranged on the tower bottom withdrawal port (104) and connected with a reboiler (11), a tower bottom reflux port is further arranged at the bottom of the first recovery tower (1), a reflux pipe is arranged on the reboiler (11) and connected with the tower bottom reflux port, a withdrawal line is further arranged on the reboiler (11) and connected with an extraction solvent condenser (12), and the extraction solvent condenser (12) is connected with an extraction solvent lateral line inlet (106) through the withdrawal line.
3. The double-partition extractive distillation column of claim 1, wherein: an extraction solvent supplement line (109) is also arranged on a withdrawal line between the extraction solvent condenser (12) and the extraction solvent side inlet (106).
4. The double-partition extractive distillation column of claim 1, wherein: a withdrawal line is arranged on the second mixed liquid side line withdrawal port (102) and connected with a second mixed liquid condenser (4), the second mixed liquid condenser (4) is connected with a second mixed liquid reflux tank (5), a reflux port is further arranged at the top of the first recovery tower (1), a reflux pipe is arranged on the second mixed liquid reflux tank (5) and connected with the reflux port, and a withdrawal line is further arranged on the second mixed liquid reflux tank (5) and connected with a second mixed liquid side line inlet (107).
5. The double-partition extractive distillation column of claim 1, wherein: an extraction line is arranged at the second product extraction outlet (105) and is connected with a second product condenser (7), the second product condenser (7) is connected with a second product reflux tank (8), a second product reflux port is further arranged at the top of the extraction rectifying tower (2), a reflux pipe is arranged on the second product reflux tank (8) and is connected with the second product reflux port, and a second product extraction line is further arranged on the second product reflux tank (8).
6. The double-partition extractive distillation column of claim 1, wherein: a third product side line extraction outlet (108) is provided with an extraction line connected with a third product condenser (9), the third product condenser (9) is connected with a third product reflux tank (10), the top of the third product recovery tower (3) is also provided with a third product reflux opening, the third product reflux tank (10) is provided with a reflux pipe connected with the third product reflux opening, and the third product reflux tank (10) is also provided with a third product extraction line.
7. The double-partition extractive distillation column of claim 1, wherein: the number of theoretical plates of the first recovery tower (1) is 38-42, the first mixed liquid inlet (101) is positioned at 8-12 plates, the first product side draw outlet (103) is positioned at 23-27 plates, the first passage (A) is positioned at 30-34 plates, the rectifying section is positioned between 1-10 plates, the dehydrating section is positioned between 10-32 plates, and the stripping section is positioned between 32-40 plates.
8. The double-partition extractive distillation column of claim 1, wherein: the theoretical plate number of the second recovery tower (2) is 38-42, the side inlet (106) of the extraction solvent is positioned at 3-5 plates, the side inlet (107) of the second mixed liquid is positioned at 23-27 plates, and the fourth passage (D) is positioned at the bottommost part of the second recovery tower (2).
9. The double-partition extractive distillation column of claim 1, wherein: the theoretical plate number of the third recovery tower (3) is 38-42, the third channel (C) is positioned at 23-27 plates, and the fourth channel (B) is positioned at the bottommost part of the methanol recovery tower (3).
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