CN112843765A - Micro-scale efficient rectification separation process strengthening device and process - Google Patents

Micro-scale efficient rectification separation process strengthening device and process Download PDF

Info

Publication number
CN112843765A
CN112843765A CN202011393123.8A CN202011393123A CN112843765A CN 112843765 A CN112843765 A CN 112843765A CN 202011393123 A CN202011393123 A CN 202011393123A CN 112843765 A CN112843765 A CN 112843765A
Authority
CN
China
Prior art keywords
micro
rectification
flow
column
separation process
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN202011393123.8A
Other languages
Chinese (zh)
Other versions
CN112843765B (en
Inventor
高鑫
王佳硕
李洪
李鑫钢
从海峰
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Tianjin University
Original Assignee
Tianjin University
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Tianjin University filed Critical Tianjin University
Priority to CN202011393123.8A priority Critical patent/CN112843765B/en
Publication of CN112843765A publication Critical patent/CN112843765A/en
Application granted granted Critical
Publication of CN112843765B publication Critical patent/CN112843765B/en
Expired - Fee Related legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Classifications

    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D3/00Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/14Fractional distillation or use of a fractionation or rectification column
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D3/00Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/14Fractional distillation or use of a fractionation or rectification column
    • B01D3/32Other features of fractionating columns ; Constructional details of fractionating columns not provided for in groups B01D3/16 - B01D3/30
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C29/00Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
    • C07C29/74Separation; Purification; Use of additives, e.g. for stabilisation
    • C07C29/76Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
    • C07C29/80Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C7/00Purification; Separation; Use of additives
    • C07C7/04Purification; Separation; Use of additives by distillation
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D2202/00Details concerning evaporation, distillation or condensation
    • B01D2202/10Use of a microdevice for separation

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Analytical Chemistry (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Water Supply & Treatment (AREA)
  • Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)

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

Micro-scale efficient rectification separation process strengthening device and process
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)

1.一种微尺度高效精馏分离过程强化装置,其特征在于:包括进料管、进料蠕动泵、换热器、微精馏柱、冷凝器、限域流动微结构及再沸器,所述进料管连接至所述进料蠕动泵,所述进料蠕动泵通过输料管连接至所述换热器,所述换热器连接至所述微精馏柱的进料口,所述微精馏柱顶部的气相出口通过管路连接至所述冷凝器,所述冷凝器上设置有回流口及顶端物料采出口,所述回流口连接至所述微精馏柱顶部的回流口,所述回流口连接至限域流动微结构上端,所述限域流动微结构下端通过固定头与所述微精馏柱的液相出口相连,所述微精馏柱液相出口分别连接至再沸器及底端物料采出口,所述再沸器连接至所述微精馏柱。1. a micro-scale high-efficiency rectification separation process strengthening device, is characterized in that: comprise feed pipe, feed peristaltic pump, heat exchanger, micro-rectification column, condenser, restricted flow microstructure and reboiler, The feed pipe is connected to the feed peristaltic pump, and the feed peristaltic pump is connected to the heat exchanger through the feed pipe, and the heat exchanger is connected to the feed port of the micro-rectification column, The gas phase outlet at the top of the micro-rectification column is connected to the condenser through a pipeline, and the condenser is provided with a reflux port and a top material extraction port, and the reflux port is connected to the reflux at the top of the micro-rectification column. The return port is connected to the upper end of the confined flow microstructure, and the lower end of the confined flow microstructure is connected to the liquid phase outlet of the micro-rectification column through a fixed head, and the liquid-phase outlet of the micro-rectification column is respectively connected To the reboiler and the bottom material extraction port, the reboiler is connected to the micro-rectification column. 2.根据权利要求1所述的微尺度高效精馏分离过程强化装置,其特征在于:所述限域流动微结构为微螺旋结构,所述微螺旋结构的螺旋内部和螺线间隙中有液相流动,所述微螺旋结构的螺旋外侧有气相流动,所述气相及液相在螺线间隙接触并传质;所述微螺旋结构的长度为10~500mm,外径为0.4~1.5mm,螺旋间隙为0.1~0.5mm,螺线截面为矩形、圆形或梯形,螺旋方向为顺时针下降或逆时针下降。2. The microscale high-efficiency rectification and separation process intensification device according to claim 1, characterized in that: the confined flow microstructure is a micro-spiral structure, and there is liquid inside the spiral of the micro-spiral structure and in the spiral gap. Phase flow, there is a gas phase flow outside the spiral of the micro-spiral structure, the gas phase and the liquid phase are in contact and mass transfer in the spiral gap; the length of the micro-spiral structure is 10-500mm, the outer diameter is 0.4-1.5mm, The spiral gap is 0.1-0.5mm, the spiral section is rectangular, circular or trapezoidal, and the spiral direction is clockwise descending or counterclockwise descending. 3.根据权利要求1所述的微尺度高效精馏分离过程强化装置,其特征在于:所述限域流动微结构为微集束结构,所述微集束结构内侧有液相流动,所述微集束结构外侧有气相流动,所述气相及液相在微集束间隙接触并传质;所述微集束结构的长度为10~500mm,外径为0.4~1.5mm,集束间距为0.1~0.5mm;集束截面为矩形或圆形。3 . The micro-scale high-efficiency rectification and separation process intensification device according to claim 1 , wherein the confined flow microstructure is a micro-bundle structure, the inner side of the micro-bundle structure has liquid flow, and the micro-bundle structure has a liquid phase flow. 4 . A gas phase flows on the outside of the structure, and the gas phase and the liquid phase contact and transfer mass in the micro-cluster gap; the length of the micro-cluster structure is 10-500mm, the outer diameter is 0.4-1.5mm, and the cluster spacing is 0.1-0.5mm; clustering The cross section is rectangular or circular. 4.根据权利要求1所述的微尺度高效精馏分离过程强化装置,其特征在于:所述限域流动微结构为微侧柱结构,所述微侧柱结构的侧柱间隙有液相流动,所述微侧柱结构的侧柱外侧有气相流动,所述气相及液相在侧柱间隙的凹液面处接触并传质;所述微侧柱结构的长度为10~500mm,外径为0.2~1.0mm,侧柱长度为0.1~0.5mm,侧柱分布角度为2~30°,侧柱截面为矩形、圆形或三角形。4. The micro-scale high-efficiency rectification separation process intensification device according to claim 1, wherein the confined flow microstructure is a micro-side column structure, and the side column gap of the micro-side column structure has a liquid phase flow , the outer side of the side pillar of the micro-side pillar structure has a gas phase flow, and the gas phase and the liquid phase contact and transfer mass at the concave liquid surface of the side pillar gap; the length of the micro side pillar structure is 10-500mm, and the outer diameter The length of the side pillar is 0.2-1.0mm, the length of the side pillar is 0.1-0.5mm, the distribution angle of the side pillar is 2-30°, and the cross-section of the side pillar is rectangular, circular or triangular. 5.根据权利要求1所述的微尺度高效精馏分离过程强化装置,其特征在于:所述限域流动微结构为微侧孔结构,所述微侧孔结构内侧有液相流动,所述微侧孔结构外侧有气相流动,所述气相及液相在侧孔处接触并传质;微侧孔结构的长度为10~500mm,外径为0.5~1.5mm,壁厚0.1~0.3mm,侧孔为圆形、矩形或三角形。5 . The micro-scale high-efficiency rectification and separation process intensification device according to claim 1 , wherein the confined flow microstructure is a micro-side pore structure, and the inner side of the micro-side pore structure has liquid flow, and the A gas phase flows on the outside of the micro-side hole structure, and the gas phase and the liquid phase contact and transfer mass at the side holes; the length of the micro-side hole structure is 10-500mm, the outer diameter is 0.5-1.5mm, and the wall thickness is 0.1-0.3mm, Side holes are round, rectangular or triangular. 6.根据权利要求1所述的微尺度高效精馏分离过程强化装置,其特征在于:所述限域流动微结构为直线型或弯曲型,操作角度为0~90°。6 . The micro-scale high-efficiency rectification and separation process intensification device according to claim 1 , wherein the confined flow microstructure is linear or curved, and the operating angle is 0-90°. 7 . 7.一种微尺度高效精馏分离过程强化工艺,其特征在于:所述工艺流程为:7. a micro-scale high-efficiency rectification separation process strengthening process, is characterized in that: described technological process is: 1)精馏进料:待精馏分离的物料通过进料管由进料蠕动泵进行输送进料;1) rectification feed: the material to be rectified and separated is transported and fed by the feed peristaltic pump through the feed pipe; 2)进料换热:进料蠕动泵输送的物料经换热器换热后生成气体混合物;2) Feed heat exchange: the material transported by the feed peristaltic pump generates a gas mixture after heat exchange by the heat exchanger; 3)精馏分离:气相混合物通过微精馏柱的进料口进入微精馏柱进行精馏,微精馏柱顶端的气相产物通过气相出口进入冷凝器,冷凝液冷凝后的液相物料一部分作为产物经顶端物料采出口采出,另一部分作为回流物料返回到微精馏柱的回流口,回流物料沿限域流动微结构向下流动,并与向上流动的气相接触传质;微精馏柱底端的液相通过液相出口流出,一部分作为产物经底端物料采出口采出,另一部分进入再沸器,经过再沸器再次加热返回微精馏柱。3) Rectification separation: the gas-phase mixture enters the micro-rectification column for rectification through the feed port of the micro-rectification column, the gas-phase product at the top of the micro-rectification column enters the condenser through the gas-phase outlet, and a part of the liquid-phase material after the condensate condenses As a product, it is extracted through the top material extraction port, and the other part is returned to the reflux port of the micro-rectification column as a reflux material. The reflux material flows down along the confined flow microstructure and contacts with the upwardly flowing gas phase for mass transfer; micro-rectification The liquid phase at the bottom of the column flows out through the liquid phase outlet, a part is extracted as a product through the material extraction outlet at the bottom, and the other part enters the reboiler, and is heated again through the reboiler to return to the micro-rectification column. 8.根据权利要求7所述的微尺度高效精馏分离过程强化工艺,其特征在于:所述进料蠕动泵的进料量为1~50μL/min。8 . The micro-scale high-efficiency rectification and separation process strengthening process according to claim 7 , wherein the feeding amount of the feeding peristaltic pump is 1-50 μL/min. 9 . 9.根据权利要求7所述的微尺度高效精馏分离过程强化工艺,其特征在于:所述换热器的出口热物流温度为50~200℃。9 . The micro-scale high-efficiency rectification separation process enhancement process according to claim 7 , wherein the temperature of the hot stream at the outlet of the heat exchanger is 50-200° C. 10 . 10.根据权利要求7所述的微尺度高效精馏分离过程强化工艺,其特征在于:所述微精馏柱的绝对压力为1~2atm,所述微精馏柱的回流比为0.5~8。10. The micro-scale high-efficiency rectification separation process strengthening process according to claim 7, wherein 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 .
CN202011393123.8A 2020-12-03 2020-12-03 Micro-scale efficient rectification separation process strengthening device and process Expired - Fee Related CN112843765B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202011393123.8A CN112843765B (en) 2020-12-03 2020-12-03 Micro-scale efficient rectification separation process strengthening device and process

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202011393123.8A CN112843765B (en) 2020-12-03 2020-12-03 Micro-scale efficient rectification separation process strengthening device and process

Publications (2)

Publication Number Publication Date
CN112843765A true CN112843765A (en) 2021-05-28
CN112843765B CN112843765B (en) 2022-04-01

Family

ID=75996877

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202011393123.8A Expired - Fee Related CN112843765B (en) 2020-12-03 2020-12-03 Micro-scale efficient rectification separation process strengthening device and process

Country Status (1)

Country Link
CN (1) CN112843765B (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113521784A (en) * 2021-07-05 2021-10-22 内蒙古工业大学 A micro-distillation heat integrated system

Citations (18)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4597947A (en) * 1983-06-30 1986-07-01 The United States Of America As Represented By The Secretary Of The Army Mass transfer and material separation microchannel plate apparatus
US20040211726A1 (en) * 2001-06-22 2004-10-28 Baig Fakhir U. Membrane-assisted fluid separation apparatus and method
US20060016215A1 (en) * 2004-07-23 2006-01-26 Tonkovich Anna L Distillation process using microchannel technology
CN1956758A (en) * 2004-05-01 2007-05-02 农业研究有限公司 Drying process and equipment
CN101668574A (en) * 2007-06-20 2010-03-10 纳格祖那能量私人有限公司 Process and apparatus for concentrating dilute solution
DE102009024801A1 (en) * 2009-05-29 2010-12-02 Siemens Aktiengesellschaft Microfluidic separator for liquid mixtures
CN102731438A (en) * 2012-06-18 2012-10-17 天津大学 Absorption-rectification method and apparatus for separation of carbon dioxide-epoxypropane mixture
CN102869439A (en) * 2010-04-30 2013-01-09 塞彭公司 Reactor for effecting gas-liquid biphasic reactions
CN103253676A (en) * 2013-05-10 2013-08-21 河北工业大学 Preparation method of trichlorosilane
CN103391799A (en) * 2010-08-10 2013-11-13 佐治亚科技研究公司 Vapor-liquid heat and/or mass exchange device
CN105457322A (en) * 2015-11-30 2016-04-06 江苏德林环保技术有限公司 Microtube distillation and condensation method and device
CN106565516A (en) * 2016-11-14 2017-04-19 成都惠恩精细化工有限责任公司 Long-chain alkyl formamide, preparation method thereof, and formylation rectification device
CN106866380A (en) * 2017-02-20 2017-06-20 河北工业大学 A kind of micro- reactive distillation plate prepares the method and its equipment of 2,6 BHTs
CN107903165A (en) * 2017-10-25 2018-04-13 常州大学 A kind of method that m-methyl benzoic acid is continuously prepared using tubular reactor
CN108371825A (en) * 2018-05-04 2018-08-07 吉林北沙制药有限公司 A kind of mocromembrane evaporator, the distillation system comprising mocromembrane evaporator and the rectificating method using mocromembrane evaporator
CN108579116A (en) * 2018-07-03 2018-09-28 衢州市鼎盛化工科技有限公司 A kind of bead tube, rectifying column and rectifying plate
CN109569002A (en) * 2018-12-31 2019-04-05 江西石华精细化工科技协同创新有限公司 A kind of method of extensive purification trimethyl aluminium crude product
CN111269080A (en) * 2020-02-20 2020-06-12 扬州虹扬科技发展有限公司 A kind of microreactor preparation system of perfluoro 1,3-butadiene and preparation method thereof

Patent Citations (19)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4597947A (en) * 1983-06-30 1986-07-01 The United States Of America As Represented By The Secretary Of The Army Mass transfer and material separation microchannel plate apparatus
US20040211726A1 (en) * 2001-06-22 2004-10-28 Baig Fakhir U. Membrane-assisted fluid separation apparatus and method
CN1956758A (en) * 2004-05-01 2007-05-02 农业研究有限公司 Drying process and equipment
US20060016215A1 (en) * 2004-07-23 2006-01-26 Tonkovich Anna L Distillation process using microchannel technology
CN101035601A (en) * 2004-07-23 2007-09-12 万罗赛斯公司 Distillation process using microchannel technology
CN101668574A (en) * 2007-06-20 2010-03-10 纳格祖那能量私人有限公司 Process and apparatus for concentrating dilute solution
DE102009024801A1 (en) * 2009-05-29 2010-12-02 Siemens Aktiengesellschaft Microfluidic separator for liquid mixtures
CN102869439A (en) * 2010-04-30 2013-01-09 塞彭公司 Reactor for effecting gas-liquid biphasic reactions
CN103391799A (en) * 2010-08-10 2013-11-13 佐治亚科技研究公司 Vapor-liquid heat and/or mass exchange device
CN102731438A (en) * 2012-06-18 2012-10-17 天津大学 Absorption-rectification method and apparatus for separation of carbon dioxide-epoxypropane mixture
CN103253676A (en) * 2013-05-10 2013-08-21 河北工业大学 Preparation method of trichlorosilane
CN105457322A (en) * 2015-11-30 2016-04-06 江苏德林环保技术有限公司 Microtube distillation and condensation method and device
CN106565516A (en) * 2016-11-14 2017-04-19 成都惠恩精细化工有限责任公司 Long-chain alkyl formamide, preparation method thereof, and formylation rectification device
CN106866380A (en) * 2017-02-20 2017-06-20 河北工业大学 A kind of micro- reactive distillation plate prepares the method and its equipment of 2,6 BHTs
CN107903165A (en) * 2017-10-25 2018-04-13 常州大学 A kind of method that m-methyl benzoic acid is continuously prepared using tubular reactor
CN108371825A (en) * 2018-05-04 2018-08-07 吉林北沙制药有限公司 A kind of mocromembrane evaporator, the distillation system comprising mocromembrane evaporator and the rectificating method using mocromembrane evaporator
CN108579116A (en) * 2018-07-03 2018-09-28 衢州市鼎盛化工科技有限公司 A kind of bead tube, rectifying column and rectifying plate
CN109569002A (en) * 2018-12-31 2019-04-05 江西石华精细化工科技协同创新有限公司 A kind of method of extensive purification trimethyl aluminium crude product
CN111269080A (en) * 2020-02-20 2020-06-12 扬州虹扬科技发展有限公司 A kind of microreactor preparation system of perfluoro 1,3-butadiene and preparation method thereof

Non-Patent Citations (6)

* Cited by examiner, † Cited by third party
Title
(葡)阿丰索等: "《绿色分离过程 基础与应用》", 31 May 2008, 华东理工大学出版社 *
CC LIU,ET AL.: "Micro-Distillation System for Formaldehyde Concentration Detection", 《THE CHEMICAL ENGINEERING JOURNAL》 *
CONG H , LI X , HONG L , ET AL.: "Performance Analysis and Structural Optimization of Multi-Tube Type Heat Integrated Distillation Column (HIDiC)", 《SEPARATION AND PURIFICATION TECHNOLOGY》 *
CONG H , ZHAO Z , LI X , ET AL.: "Liquid‐bridge flow in the channel of helical string and its application to gas–liquid contacting process", 《 BIOTECHNOLOGY PROGRESS》 *
周海鹰, 李鑫钢, 肖坤林,等: "微孔介质塔板流体力学和传质性能的研究", 《精细化工中间体》 *
李苏雅: "精密精馏气液传质机理及强化方法研究", 《工程科技Ⅰ辑》 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113521784A (en) * 2021-07-05 2021-10-22 内蒙古工业大学 A micro-distillation heat integrated system
CN113521784B (en) * 2021-07-05 2023-01-06 内蒙古工业大学 Micro-rectification heat integration system

Also Published As

Publication number Publication date
CN112843765B (en) 2022-04-01

Similar Documents

Publication Publication Date Title
CN204710289U (en) A kind of bubble tower gas-liquid reactor
CN112843765B (en) Micro-scale efficient rectification separation process strengthening device and process
CN108579116A (en) A kind of bead tube, rectifying column and rectifying plate
CN101219927B (en) Benzyl chloride structured packing column continuous separation method and device
CN101380562A (en) Window diversion type regular packing slice and packing material
CN106390503B (en) A kind of gasket packing rectifying column
WO1996006665A1 (en) Internal heat exchange type distillation column
CN220125529U (en) Distilling device for sample detection
CN100465147C (en) Fractionating tower for separating acrylic aldehyde from 3-hydroxypropionaldehyde solution
CN102512962A (en) Multi-tube pass inorganic separating membrane module
US9259705B2 (en) Microreactor device having an essentially vertical or inclined upper portion comprising means for collection and removal of gas formed in situ during a liquid-medium reaction and method
CN218529831U (en) Device for rectifying and separating acetone water by supergravity
CN116650988A (en) Micro-rectification device and method for efficiently separating near-boiling-point mixture
CN219441642U (en) Microchannel reaction structure convenient to wash
CN206626991U (en) A kind of close-coupled micro-channel heat exchanger
CN113583032B (en) Cracking device and method for boron trifluoride complex
CN112174816B (en) Method and device for reactive distillation and membrane coupling in backpack tower
CN208525866U (en) A kind of bead tube, rectifying column and rectifying plate
CN212347770U (en) Rectifying tower for high-speed high-recovery-rate purification
JP2732373B2 (en) Internal heat exchange distillation column
CN206746525U (en) A kind of self-catalysis microreactor channel design
CN118203867B (en) Multistage rectification system of fluoroethylene carbonate
CN201551865U (en) Rectifying tower
CN113521784B (en) Micro-rectification heat integration system
CN221732414U (en) A new type of acetonitrile decyanation tower

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant
CF01 Termination of patent right due to non-payment of annual fee
CF01 Termination of patent right due to non-payment of annual fee

Granted publication date: 20220401