CN112843765A - Micro-scale efficient rectification separation process strengthening device and process - Google Patents
Micro-scale efficient rectification separation process strengthening device and process Download PDFInfo
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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
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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
- B01D3/32—Other features of fractionating columns ; Constructional details of fractionating columns not provided for in groups B01D3/16 - B01D3/30
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- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
- C07C29/80—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation
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- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C7/00—Purification; Separation; Use of additives
- C07C7/04—Purification; Separation; Use of additives by distillation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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Abstract
The invention relates to a device and a process for strengthening a micro-scale efficient rectification separation process. The microscale high-efficiency rectification separation process strengthening device utilizes the constraint of various limited-domain flow microstructures to guide the liquid phase to flow, and the gas phase flows outside the limited-domain flow microstructures, so that the rectification separation process strengthening of gas-liquid two-phase reverse flow mass transfer under microscale is realized, the gas-liquid mass transfer efficiency is greatly promoted, and the microscale high-efficiency rectification separation process strengthening device can be applied to the separation and purification process of high-purity chemicals. The method and the device for strengthening the micro-scale efficient rectification separation process have simple structure and easy manufacture, can effectively separate the mixture with a near boiling point, and can obtain theoretical plates with the plate height of 5-13 mm.
Description
Technical Field
The invention belongs to the technical field of separation and purification processes of high-purity chemicals, and relates to a device for strengthening a mass transfer separation process by high-efficiency gas/liquid phase reverse flow, in particular to a device and a process for strengthening a micro-scale high-efficiency rectification separation process.
Background
Rectification refers to a process for separating components from a miscible fluid mixture based on differences in volatility. The rectification process is simple to operate, the principle popularization rate is high, a target product with higher purity can be directly obtained, the application range is wide, and over 70 percent of the chemical separation process adopts rectification technology. However, the rectification process also has major disadvantages and shortcomings, such as large equipment, large energy consumption, difficult separation of a system with low relative volatility, and the like. The main reason is that the mass transfer is carried out on a macroscopic scale in the traditional rectification process, so the mass transfer resistance is large and the mass transfer rate is low.
As a process enhancement, microchemical techniques have many advantages, including reduced line size, large specific surface area, small volume, high heat and mass transfer rates, and the like. The rectification process is carried out in a microscale device, so that the mass transfer distance can be effectively reduced, the specific surface area is increased, and the size of the device is reduced.
The patent CN109569003A and CN109569002A propose to purify the trimethylaluminum crude product by using a microchannel rectification tower, and the related microchannel rectification tower can only be used for batch rectification, but cannot perform a continuous rectification process.
Patent US20060016215A achieves process intensification by using stacks of material sheets with stamped or etched channels that provide narrow flow paths with short diffusion distances for mass transfer. However, the liquid phase distribution is difficult, and the short circuit phenomenon is easy to occur. The gas-liquid phase adopts a parallel flow mode, and the best separation performance which can be achieved is only one theoretical level. A porous membrane (ZhangY, axial. vacuum membrane distillation by microchip with temperature gradient) is used to maintain a gas-liquid phase interface for the micro-scale rectification process, and carrier gas or vacuum is required to generate a pressure difference to drive the fluid. The phase interface of gas-liquid countercurrent contact can be established by centrifugal force (macroins, et al. experimental neutralization of rotating spiral microchannel), but the operation is complicated and is not suitable for large-scale application. The application of capillary forces (Lam, et al. development of a microfluidic chip) relies on the design of capillary structures, some of which are time consuming and laborious. The development and design of a structure which is simple in manufacture and high-efficiency and can realize gas-liquid countercurrent flow contact mass transfer, and a microscale rectification method and a microscale rectification device are urgently needed.
Disclosure of Invention
The invention aims to provide a device and a process for strengthening a micro-scale efficient rectification separation process, aiming at the defects and the defects of the prior art.
The technical problem to be solved by the invention is realized by the following technical scheme:
a microscale high-efficiency rectification separation process strengthening device is characterized in that: including inlet pipe, feeding peristaltic pump, heat exchanger, little rectifying column, condenser, confined flow microstructure and reboiler, the inlet pipe is connected to the feeding peristaltic pump, the feeding peristaltic pump is connected to through the conveying pipeline the heat exchanger, the heat exchanger is connected to the feed inlet of little rectifying column, the gaseous phase export at little rectifying column top is through tube coupling to the condenser, be provided with backward flow mouth and top material extraction outlet on the condenser, the backward flow mouth is connected to the backward flow mouth at little rectifying column top, the backward flow mouth is connected to confined flow microstructure upper end, confined flow microstructure lower extreme through the fixed head with the liquid phase export of little rectifying column links to each other, little rectifying column liquid phase export is connected to reboiler and bottom material extraction outlet respectively, the reboiler is connected to little rectifying column.
The confined flow microstructure is a micro-spiral structure, liquid phase flows in the spiral inner part and the spiral gaps of the micro-spiral structure, gas phase flows outside the spiral of the micro-spiral structure, and the gas phase and the liquid phase are contacted and transfer mass in the spiral gaps; the length of the micro-spiral structure is 10-500 mm, the outer diameter is 0.4-1.5 mm, the spiral gap is 0.1-0.5 mm, the cross section of the spiral line is rectangular, circular or trapezoidal, and the spiral direction descends clockwise or anticlockwise.
The micro-cluster structure is characterized in that the confined flow microstructure is a micro-cluster structure, liquid phase flows inside the micro-cluster structure, gas phase flows outside the micro-cluster structure, and the gas phase and the liquid phase are contacted and mass-transferred in a micro-cluster gap; the length of the micro cluster structure is 10-500 mm, the outer diameter is 0.4-1.5 mm, and the cluster spacing is 0.1-0.5 mm; the cross section of the bundling is rectangular or circular.
Moreover, the confined flow microstructure is a micro side column structure, a liquid phase flows in a side column gap of the micro side column structure, a gas phase flows outside a side column of the micro side column structure, and the gas phase and the liquid phase are contacted at a concave liquid surface of the side column gap and transfer mass; the length of little side post structure is 10 ~ 500mm, and the external diameter is 0.2 ~ 1.0mm, and side post length is 0.1 ~ 0.5mm, and the side post distribution angle is 2 ~ 30, and the side post cross-section is rectangle, circular or triangle-shaped.
Moreover, the limited-area flow microstructure is a micro side hole structure, liquid phase flows inside the micro side hole structure, gas phase flows outside the micro side hole structure, and the gas phase and the liquid phase are contacted and transfer mass at the side holes; the length of the micro side hole structure is 10-500 mm, the outer diameter is 0.5-1.5 mm, the wall thickness is 0.1-0.3 mm, and the side holes are circular, rectangular or triangular.
Moreover, the restricted flow microstructure is linear or curved, and the operating angle is 0-90 degrees.
A micro-scale efficient rectification separation process strengthening process is characterized in that: the process flow comprises the following steps:
1) and (3) rectification feeding: the material to be rectified and separated is conveyed and fed by a feeding peristaltic pump through a feeding pipe;
2) feeding and heat exchange: the material conveyed by the feeding peristaltic pump generates a gas mixture after heat exchange by the heat exchanger;
3) rectification and separation: the gas phase mixture enters the micro-rectification column through a feed inlet of the micro-rectification column for rectification, a gas phase product at the top end of the micro-rectification column enters a condenser through a gas phase outlet, one part of a liquid phase material condensed by the condensate liquid is taken out through a top material extraction port as a product, the other part of the liquid phase material is taken as a backflow material and returns to a backflow port of the micro-rectification column, and the backflow material flows downwards along the confined flow microstructure and is in contact mass transfer with the gas phase flowing upwards; and the liquid phase at the bottom end of the micro-rectification column flows out through a liquid phase outlet, one part of the liquid phase is taken as a product and is extracted through a bottom material extraction port, and the other part of the liquid phase enters a reboiler and is heated again through the reboiler and returns to the micro-rectification column.
And the feeding amount of the feeding peristaltic pump is 1-50 mu L/min.
And the temperature of the outlet hot material flow of the heat exchanger is 50-200 ℃.
The absolute pressure of the micro-rectification column is 1 to 2atm, and the reflux ratio of the micro-rectification column is 0.5 to 8.
The invention has the advantages and beneficial effects that:
1. the reinforcing device for the micro-scale efficient rectification separation process utilizes the constraint of various limited-area flow microstructures to guide the liquid phase to flow, and the gas phase flows outside the microstructures, so that the reinforcing device realizes the reinforcement of the rectification separation process of gas-liquid phase reverse flow and mass transfer in the micro-scale device, reduces the volume of the device, shortens the mass transfer distance, greatly promotes the gas-liquid mass transfer efficiency, and is safer to operate.
2. The strengthening process and the device for the micro-scale efficient rectification separation process have simple structures and easy manufacture, and can obtain 99.9% purity acetone when separating an acetone-n-butanol mixture, the height of a theoretical plate and the like reaches 5mm, the mixture with a near boiling point can be effectively separated, and the height of the obtained theoretical plate and the like reaches 5-13 mm.
Drawings
FIG. 1 is a schematic vertical operation of the microscale enhanced apparatus for efficient distillation and separation of the present invention;
FIG. 2 is a schematic diagram of a horizontal operation of the micro-scale high efficiency distillation separation process enhancement apparatus of the present invention;
FIG. 3 is a schematic structural view of a micro-helix structure according to the present invention;
FIG. 4 is a schematic structural diagram of a micro-cluster structure according to the present invention;
FIG. 5 is a schematic structural view of a micro-pillar structure according to the present invention;
FIG. 6 is a schematic structural view of a micro-lateral hole structure according to the present invention.
Detailed Description
The present invention is further illustrated by the following specific examples, which are intended to be illustrative, not limiting and are not intended to limit the scope of the invention.
Example 1
The device of the invention is used for separating equimolar hexane-cyclohexane mixture, as shown in figure 1, and comprises a feed peristaltic pump (2), a heat exchanger (4), a micro-rectification column (6), a condenser (8), a confined flow microstructure (13) and a reboiler (18); the micro-spiral structure shown in figure 3 is selected as the zone-limited flow microstructure (13), the cross section of the spiral is rectangular, the spiral direction is anticlockwise reduced, the length is 80mm, the outer diameter is 0.50mm, the spiral gap is 0.25mm, the width of the spiral is 0.10mm, and the thickness of the spiral is 0.10 mm.
A hexane-cyclohexane mixture to be separated enters a heat exchanger (4) from a feeding pipe (1) through a feeding peristaltic pump (2) and a conveying pipe (3), a generated gas mixture (5) enters a micro-rectifying column (6) through a feeding hole of the micro-rectifying column, a gas-phase product (7) rich in high-volatility substances enters a condenser (8), a part of material (10) of a condensed liquid-phase material (9) is extracted, a rest material (11) flows back to the micro-rectifying column (6) through a backflow hole (12), flows from top to bottom along a limited-area flow microstructure (13), flows out of the micro-rectifying column (6) through a fixed head (14), a part of material (16) of a material (15) at the bottom of the micro-rectifying column is extracted, a rest material (17) enters a reboiler (18), and a hot material (19) reheated by the reboiler (18) returns to the micro-rectifying column.
The feeding amount of the feeding peristaltic pump (2) is 1uL/min, the outlet hot material flow temperature of the heat exchanger (4) is 74 ℃, the absolute pressure of the micro-rectification column (6) is 1.2atm, and the reflux ratio of the micro-rectification column is 4.
After the above process, the molar concentration of hexane at the top of the column was 0.83, the molar concentration of hexane at the bottom of the column was 0.15, and the theoretical plate height was 8.8 mm.
Example 2
The device is used for separating an equimolar acetone-n-butanol mixture, and comprises a feeding peristaltic pump (2), a heat exchanger (4), a micro rectifying column (6), a condenser (8), a limited-area flow microstructure (13) and a reboiler (18) as shown in figure 1; the micro cluster structure shown in figure 4 is selected as the zone-limited flow microstructure (13), the cluster cross section is circular, the diameter is 0.02mm, the length of the microstructure is 20mm, the outer diameter is 0.8mm, and the fixed interval is 10 mm. The acetone-n-butanol mixture to be separated enters a heat exchanger (4) through a feeding peristaltic pump (2), a generated gas mixture (5) enters a micro-rectification column (6) through a micro-rectification column feeding hole, a gas phase product (7) rich in high-volatility substances enters a condenser (8), a part of materials (10) of a condensed liquid phase material (9) are extracted, the rest materials (11) flow back to the micro-rectification column (6) through a backflow hole (12), flow from top to bottom along a limited flow microstructure (13) and flow out of the micro-rectification column (6) through a fixed head (14), a part of materials (16) of a micro-rectification column bottom material (15) are extracted, and the rest materials (17) return to the micro-rectification column through a reboiler (18).
The feeding amount of the feeding peristaltic pump (2) is 15uL/min, the outlet hot material flow temperature of the heat exchanger (4) is 95 ℃, the absolute pressure of the micro-rectification column (6) is 1atm, and the reflux ratio of the micro-rectification column is 0.5.
After the above process, the molar concentration of acetone at the top of the column was 0.999, the molar concentration of acetone at the bottom of the column was 0.005, and the height of the theoretical plate was 5 mm.
Example 3
The device is used for separating an equimolar methanol-toluene mixture, and comprises a feed peristaltic pump (2), a heat exchanger (4), a micro-rectification column (6), a condenser (8), a restricted flow microstructure (13) and a reboiler (18) as shown in figure 1; the micro side pillar structure shown in figure 5 is selected as the limited area flow microstructure (13), the cross section of the side pillar is circular, the diameter is 0.03mm, the length is 0.1mm, the interval L is 0.07mm, the distribution angle is 24 degrees, the diameter of the microstructure is 0.2mm, and the length is 30 mm. A methanol-toluene mixture to be separated enters a heat exchanger (4) through a feeding peristaltic pump (2), generated gas (5) enters a micro-rectification column (6) through a feeding hole of the micro-rectification column, a gas-phase product (7) rich in high-volatility substances enters a condenser (8), a part of material (10) of a condensed liquid material (9) is extracted, the rest material (11) flows back to the micro-rectification column (6) through a backflow port (12), flows from top to bottom along a limited-area flow microstructure (13), flows out of the micro-rectification column (6) through a fixed head (14), a part of material (16) of a material (15) at the bottom of the micro-rectification column is extracted, and the rest material (17) returns to the micro-rectification column through a reboiler (18).
The feeding amount of the feeding peristaltic pump (2) is 40uL/min, the outlet hot material flow temperature of the heat exchanger (4) is 85 ℃, the absolute pressure of the micro-rectification column (6) is 1atm, and the reflux ratio of the micro-rectification column is 5.
After the above process, the molar concentration of methanol at the top of the column was 0.86, the molar concentration of methanol at the bottom of the column was 0.01, and the theoretical plate height was 6 mm.
Example 4
The device is used for separating an equimolar hexene-hexane mixture, and comprises a feeding peristaltic pump (2), a heat exchanger (4), a micro-rectification chip (7), a limited-area flow microstructure (8), a condenser (11), a reflux peristaltic pump (15), an extraction peristaltic pump (20) and a reboiler (22) as shown in figure 2; the limited area flow microstructure (8) adopts a micro side hole structure as shown in fig. 6, the section of a side hole is circular, the diameter of the side hole is 0.1mm, the interval L is 0.13mm, the distribution angle is 24 degrees, the operation angle is 0 degree, the limited area flow microstructure is a bent snake shape, and the length is 300 mm. The method comprises the steps that a hexene-hexane mixture to be separated enters a heat exchanger (4) through a feeding peristaltic pump (2), generated gas (5) enters a micro-rectification chip (7) through a micro-rectification chip feeding hole (6), a micro-rectification chip cold end material (10) enters a micro-rectification chip condenser (11) through a gas phase outlet (9), a part of condensed liquid phase material (12) is extracted, the rest material (14) flows back to a backflow port (17) of the micro-rectification chip (7) through a backflow peristaltic pump (15), flows from right to left along a confined flow microstructure (8), flows out from a liquid phase outlet (18), the micro-rectification chip (7) is extracted through a pumping peristaltic pump (20), a part of micro-rectification chip hot end material (21) is extracted, and the rest material (23) returns to the micro-rectification chip through a reboiler (24).
The feeding amount of the feeding peristaltic pump (2) is 20uL/min, the outlet hot material flow temperature of the heat exchanger (4) is 62.4 ℃, the absolute pressure of the micro-rectification chip (7) is 1atm, and the reflux ratio of the micro-rectification chip is 8.
After the process, the molar concentration of hexene in the cold end material is 0.90, the molar concentration of hexene in the hot end material is 0.075, and the height of theoretical plates and the like is 13 mm.
Although the embodiments of the present invention and the accompanying drawings are disclosed for illustrative purposes, those skilled in the art will appreciate that: various substitutions, changes and modifications are possible without departing from the spirit and scope of the invention and the appended claims, and therefore the scope of the invention is not limited to the disclosure of the embodiments and the accompanying drawings.
Claims (10)
1. A microscale high-efficiency rectification separation process strengthening device is characterized in that: including inlet pipe, feeding peristaltic pump, heat exchanger, little rectifying column, condenser, confined flow microstructure and reboiler, the inlet pipe is connected to the feeding peristaltic pump, the feeding peristaltic pump is connected to through the conveying pipeline the heat exchanger, the heat exchanger is connected to the feed inlet of little rectifying column, the gaseous phase export at little rectifying column top is through tube coupling to the condenser, be provided with backward flow mouth and top material extraction outlet on the condenser, the backward flow mouth is connected to the backward flow mouth at little rectifying column top, the backward flow mouth is connected to confined flow microstructure upper end, confined flow microstructure lower extreme through the fixed head with the liquid phase export of little rectifying column links to each other, little rectifying column liquid phase export is connected to reboiler and bottom material extraction outlet respectively, the reboiler is connected to little rectifying column.
2. The micro-scale efficient distillation separation process enhancement device according to claim 1, wherein: the limited domain flow microstructure is a micro-spiral structure, liquid phase flows in the spiral inner part and the spiral gap of the micro-spiral structure, gas phase flows outside the spiral of the micro-spiral structure, and the gas phase and the liquid phase are contacted and transfer mass in the spiral gap; the length of the micro-spiral structure is 10-500 mm, the outer diameter is 0.4-1.5 mm, the spiral gap is 0.1-0.5 mm, the cross section of the spiral line is rectangular, circular or trapezoidal, and the spiral direction descends clockwise or anticlockwise.
3. The micro-scale efficient distillation separation process enhancement device according to claim 1, wherein: the limited area flow microstructure is a micro-cluster structure, liquid phase flows inside the micro-cluster structure, gas phase flows outside the micro-cluster structure, and the gas phase and the liquid phase are contacted and mass-transferred in a micro-cluster gap; the length of the micro cluster structure is 10-500 mm, the outer diameter is 0.4-1.5 mm, and the cluster spacing is 0.1-0.5 mm; the cross section of the bundling is rectangular or circular.
4. The micro-scale efficient distillation separation process enhancement device according to claim 1, wherein: the limited-area flow microstructure is a micro side column structure, a liquid phase flows in a side column gap of the micro side column structure, a gas phase flows outside a side column of the micro side column structure, and the gas phase and the liquid phase are contacted and transfer mass at a concave liquid level in the side column gap; the length of little side post structure is 10 ~ 500mm, and the external diameter is 0.2 ~ 1.0mm, and side post length is 0.1 ~ 0.5mm, and the side post distribution angle is 2 ~ 30, and the side post cross-section is rectangle, circular or triangle-shaped.
5. The micro-scale efficient distillation separation process enhancement device according to claim 1, wherein: the limited-area flow microstructure is a micro side hole structure, liquid phase flows inside the micro side hole structure, gas phase flows outside the micro side hole structure, and the gas phase and the liquid phase are contacted and transfer mass at the side holes; the length of the micro side hole structure is 10-500 mm, the outer diameter is 0.5-1.5 mm, the wall thickness is 0.1-0.3 mm, and the side holes are circular, rectangular or triangular.
6. The micro-scale efficient distillation separation process enhancement device according to claim 1, wherein: the restricted flow microstructure is linear or bent, and the operating angle is 0-90 degrees.
7. A micro-scale efficient rectification separation process strengthening process is characterized in that: the process flow comprises the following steps:
1) and (3) rectification feeding: the material to be rectified and separated is conveyed and fed by a feeding peristaltic pump through a feeding pipe;
2) feeding and heat exchange: the material conveyed by the feeding peristaltic pump generates a gas mixture after heat exchange by the heat exchanger;
3) rectification and separation: the gas phase mixture enters the micro-rectification column through a feed inlet of the micro-rectification column for rectification, a gas phase product at the top end of the micro-rectification column enters a condenser through a gas phase outlet, one part of a liquid phase material condensed by the condensate liquid is taken out through a top material extraction port as a product, the other part of the liquid phase material is taken as a backflow material and returns to a backflow port of the micro-rectification column, and the backflow material flows downwards along the confined flow microstructure and is in contact mass transfer with the gas phase flowing upwards; and the liquid phase at the bottom end of the micro-rectification column flows out through a liquid phase outlet, one part of the liquid phase is taken as a product and is extracted through a bottom material extraction port, and the other part of the liquid phase enters a reboiler and is heated again through the reboiler and returns to the micro-rectification column.
8. The micro-scale high-efficiency rectification separation process strengthening process according to claim 7, characterized in that: the feeding amount of the feeding peristaltic pump is 1-50 mu L/min.
9. The micro-scale high-efficiency rectification separation process strengthening process according to claim 7, characterized in that: the outlet hot stream temperature of the heat exchanger is 50-200 ℃.
10. The micro-scale high-efficiency rectification separation process strengthening process according to claim 7, characterized in that: the absolute pressure of the micro-rectification column is 1-2 atm, and the reflux ratio of the micro-rectification column is 0.5-8.
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