CN114768637A - Continuous countercurrent device based on micro-dispersion technology - Google Patents
Continuous countercurrent device based on micro-dispersion technology Download PDFInfo
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- 239000006185 dispersion Substances 0.000 title claims abstract description 25
- 238000005516 engineering process Methods 0.000 title claims abstract description 16
- 238000000605 extraction Methods 0.000 claims abstract description 36
- 238000010521 absorption reaction Methods 0.000 claims abstract description 28
- 239000007788 liquid Substances 0.000 claims abstract description 22
- 238000000034 method Methods 0.000 claims abstract description 21
- 238000005086 pumping Methods 0.000 claims description 12
- 239000012528 membrane Substances 0.000 claims description 6
- 238000012546 transfer Methods 0.000 abstract description 18
- 239000012071 phase Substances 0.000 description 244
- KBPLFHHGFOOTCA-UHFFFAOYSA-N 1-Octanol Chemical compound CCCCCCCCO KBPLFHHGFOOTCA-UHFFFAOYSA-N 0.000 description 37
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 29
- 239000000243 solution Substances 0.000 description 25
- TVMXDCGIABBOFY-UHFFFAOYSA-N n-Octanol Natural products CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 description 18
- 239000007864 aqueous solution Substances 0.000 description 13
- 230000001105 regulatory effect Effects 0.000 description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 9
- 239000007791 liquid phase Substances 0.000 description 8
- CRVGTESFCCXCTH-UHFFFAOYSA-N methyl diethanolamine Chemical compound OCCN(C)CCO CRVGTESFCCXCTH-UHFFFAOYSA-N 0.000 description 8
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 238000010586 diagram Methods 0.000 description 6
- 239000007789 gas Substances 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
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- 239000000203 mixture Substances 0.000 description 4
- 238000010812 external standard method Methods 0.000 description 3
- KSSNXJHPEFVKHY-UHFFFAOYSA-N phenol;hydrate Chemical compound O.OC1=CC=CC=C1 KSSNXJHPEFVKHY-UHFFFAOYSA-N 0.000 description 3
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
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- 239000000463 material Substances 0.000 description 2
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- 238000000638 solvent extraction Methods 0.000 description 2
- PVXVWWANJIWJOO-UHFFFAOYSA-N 1-(1,3-benzodioxol-5-yl)-N-ethylpropan-2-amine Chemical compound CCNC(C)CC1=CC=C2OCOC2=C1 PVXVWWANJIWJOO-UHFFFAOYSA-N 0.000 description 1
- QMMZSJPSPRTHGB-UHFFFAOYSA-N MDEA Natural products CC(C)CCCCC=CCC=CC(O)=O QMMZSJPSPRTHGB-UHFFFAOYSA-N 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/04—Solvent extraction of solutions which are liquid
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/14—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by absorption
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/14—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by absorption
- B01D53/18—Absorbing units; Liquid distributors therefor
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D2011/002—Counter-current extraction
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D2011/005—Co-current extraction
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Abstract
The application provides a continuous countercurrent device based on a micro-dispersion technology. The device comprises: the device comprises a tubular reactor, a heavy phase inlet pipeline positioned at the upper end of the tubular reactor, and a light phase inlet pipeline positioned at the lower end of the tubular reactor; the tubular reactor is also communicated with a micro-disperser, and the upper end or the lower end of the tubular reactor is also communicated with a phase separator; and the first medium flowing from the heavy phase inlet pipeline and the second medium flowing from the light phase inlet pipeline are dispersed into micron-sized bubbles or liquid drops at a micro-disperser, and are subjected to continuous countercurrent absorption or extraction process after entering the tubular reactor, the first medium and the second medium are separated into a light phase and a heavy phase at the phase separator, the light phase flows out through a light phase outlet at the upper end of the tubular reactor, and the heavy phase flows out through a heavy phase outlet at the lower end of the tubular reactor. The method is based on a micro-dispersion technology, realizes a continuous countercurrent absorption or extraction process in the tubular reactor, and has smaller equal plate height and higher mass transfer efficiency compared with the traditional countercurrent equipment.
Description
Technical Field
The application relates to the technical field of chemistry and chemical engineering, in particular to a continuous countercurrent device based on a micro-dispersion technology.
Background
Gas-liquid absorption and liquid-liquid extraction processes, typically comprising CO, play an important role in the chemical industry2Absorption, alkali washing, hydrogen peroxide extraction and the like. Because of the existence of a two-phase equilibrium relationship of substances, a plurality of theoretical stages are often needed to meet the requirement of yield, and therefore two-phase continuous countercurrent contact devices such as sieve plate towers, packed towers and the like are often adopted. However, in the conventional absorption or extraction tower, the dispersed phase is dispersed into small droplets through a sieve plate, the size of the droplets is usually in the mm magnitude, the phenomena of coalescence, backmixing and the like occur at the inner member of the tower, the mass transfer area of two phases is small, the mass transfer efficiency is low, and a large number of tower plates or tower heights are usually required to meet the requirements.
In addition, to meet the requirements of enriching the product or reducing the solvent loss, the operation is required to be carried out under a large phase ratio (compared with more than 10), in this case, larger equipment is required, the mass transfer efficiency is low, and higher requirements are put on the mass transfer process.
Disclosure of Invention
The application provides a continuous countercurrent device based on microdispersion technique, is directed at gas-liquid absorption and liquid-liquid extraction process, realizes comparing (comparing and being greater than 10) under the operating condition extremely, can carry out the countercurrent process in conventional size tubular reactor, and then realizes multistage absorption or extraction process, improves mass transfer efficiency and is showing reduction equipment investment and running cost.
The application provides a continuous countercurrent device based on microdispersion technology, includes: a tubular reactor, a heavy phase inlet pipeline and a light phase inlet pipeline; wherein the heavy phase inlet pipeline is connected to the upper end of the tubular reactor, and the light phase inlet pipeline is connected to the lower end of the tubular reactor;
the tubular reactor is also communicated with a micro-disperser, and the upper end or the lower end of the tubular reactor is also communicated with a phase splitter;
the micro-disperser is used for micro-dispersing a first medium flowing in from the heavy phase inlet pipeline and a second medium flowing in from the light phase inlet pipeline into micron-sized bubbles or liquid drops, the micron-sized bubbles or liquid drops enter the tubular reactor to be subjected to continuous countercurrent absorption or extraction, and then are subjected to phase splitting through the phase splitter to form a light phase and a heavy phase, the light phase flows out through a light phase outlet positioned at the upper end of the tubular reactor, and the heavy phase flows out through a heavy phase outlet positioned at the lower end of the tubular reactor.
Preferably, in the case where the first medium is a continuous phase, the second medium is a dispersed phase; alternatively, where the first medium is a dispersed phase, the second medium is a continuous phase.
Preferably, when the first medium is a continuous phase, the second medium is a dispersed phase, and the micro-dispenser is connected to the light phase inlet pipe and then communicated with the tubular reactor, wherein the lower end of the tubular reactor is further connected to the micro-dispenser via a circulation pump, and the circulation pump is used for pumping the first medium flowing into the tubular reactor into the micro-dispenser.
Preferably, the phase separator is located at the upper end of the tubular reactor.
Preferably, in the case that the first medium is a dispersed phase, the second medium is a continuous phase, and the micro-dispenser is connected to the heavy phase inlet pipe and then communicated with the tubular reactor, wherein the upper end of the tubular reactor is further connected to the micro-dispenser via a circulation pump, and the circulation pump is used for pumping the second medium flowing into the tubular reactor into the micro-dispenser.
Preferably, the phase separator is located at the lower end of the tubular reactor.
Preferably, a heavy phase conveying pump is arranged on the heavy phase inlet pipeline and used for pumping the first medium into the tubular reactor; and a light phase delivery pump is arranged on the light phase inlet pipeline and is used for pumping the second medium into the tubular reactor.
Preferably, the micro-disperser refers to a membrane dispersing device or a micro-sieve dispersing device.
Preferably, the micro-sized bubbles or droplets have a size of 50-1000 μm.
Preferably, the volume ratio of the continuous phase to the dispersed phase is from 200:1 to 1: 200.
The invention provides a continuous countercurrent device based on a micro-dispersion technology, which comprises: the device comprises a tubular reactor, a heavy phase inlet pipeline positioned at the upper end of the tubular reactor, and a light phase inlet pipeline positioned at the lower end of the tubular reactor; the tubular reactor is also communicated with a micro-disperser, and the upper end or the lower end of the tubular reactor is also communicated with a phase splitter; and dispersing a first medium flowing from the heavy phase inlet pipeline and a second medium flowing from the light phase inlet pipeline into micron-sized bubbles or liquid drops at a micro-disperser, performing continuous countercurrent absorption or extraction process after the first medium and the second medium enter the tubular reactor, and performing phase separation at the phase separator to obtain a light phase and a heavy phase, wherein the light phase flows out through a light phase outlet at the upper end of the tubular reactor, and the heavy phase flows out through a heavy phase outlet at the lower end of the tubular reactor.
Compared with the prior art, the method has the following advantages:
because the micro-dispersion device can be used for forming uniform and controllable micron-sized bubbles or liquid drops based on a micro-dispersion technology, the micro-dispersion process refers to the flow mass transfer and reaction process of micro-liquid drops or micro-bubbles within the range of 10-1000 mu m, and the micro-dispersion device has excellent mass transfer performance and controllability due to the micron-sized size and the plug flow characteristic, thereby realizing the continuous countercurrent efficient absorption or extraction process in the tubular reactor based on the micro-bubbles and the micro-liquid drop micro-scale effect.
In addition, uniform and controllable micron-sized bubbles or liquid drops are formed through the micro-disperser, the specific surface area is large, and the mass transfer efficiency is high; meanwhile, the size reduction enables the ascending or sedimentation rate of the dispersed phase to be reduced, the retention time of the dispersed phase is improved, the equipment height is smaller under the same retention time requirement, and the equipment investment and the material loss are favorably saved;
again, the continuous phase achieves a micro-dispersion process with the dispersed phase through the circulation pump, enabling operation at high phase ratios (two phase volume ratios greater than 10).
Drawings
FIG. 1 is a schematic structural diagram of a continuous countercurrent device based on a microdispersion technology provided by the present application;
FIG. 2 is a schematic diagram of the apparatus of the present application in which the first medium is a continuous phase;
FIG. 3 is a schematic diagram of the structure of the device of the present application in which the first medium is a dispersed phase.
Reference numerals are as follows: a-a heavy phase inlet; b-a light phase inlet; c-a light phase outlet; a D-heavy phase outlet; e-circulating liquid; 1-a heavy phase delivery pump; 2-a light phase delivery pump; 3-a light phase outlet pump; 4-heavy phase flow regulating valve; 5-a circulating pump; 6-a micro-disperser; 7-a tubular reactor; 8-phase splitter.
Detailed Description
The present application is further illustrated by the following specific examples. It should be noted that the embodiments and features of the embodiments of the present application may be combined with each other without conflict.
In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present application. However, the present application may be practiced otherwise than as specifically described herein. Therefore, the present application is not limited to the specific embodiments disclosed in the following description.
Referring to fig. 1, a schematic structural diagram of a continuous countercurrent device based on a micro-dispersion technique is shown, and as shown in fig. 1, the continuous countercurrent device based on the micro-dispersion technique comprises: a tubular reactor 7, a heavy phase inlet pipeline 1 and a light phase inlet pipeline 2; wherein the heavy phase inlet line 1 is connected to the upper end of a tubular reactor 7 and the light phase inlet line 2 is connected to the lower end of the tubular reactor 7;
the tubular reactor 7 is also communicated with a micro-disperser 6, the upper end of the tubular reactor 7 is also communicated with a phase separator 8, and in another embodiment, the phase separator 8 can also be arranged at the lower end of the tubular reactor 7;
the micro-disperser 6 is used for micro-dispersing the first medium flowing in from the heavy phase inlet pipeline 1 and the second medium flowing in from the light phase inlet pipeline 2 into micron-sized bubbles or droplets, the micron-sized bubbles or droplets enter the tubular reactor 7 to be subjected to continuous countercurrent absorption or extraction, and then are subjected to phase separation into a light phase and a heavy phase through the phase separator 8, the light phase flows out through a light phase outlet at the upper end of the tubular reactor 7, and the heavy phase flows out through a heavy phase outlet at the lower end of the tubular reactor 7.
Wherein, the light phase refers to the fluid of the one-phase with lower density, and the heavy phase refers to the fluid of the one-phase with higher density.
In specific implementation, a circulating pump is further communicated between the micro-disperser 6 and the tubular reactor 7, under the condition that the first medium is a continuous phase and the second medium is a dispersed phase, the micro-disperser 6 can be communicated with the tubular reactor 7 after being connected with the light phase inlet pipeline 2, and the phase separator 8 is positioned at the upper end of the tubular reactor 7; in the case where the first medium is a dispersed phase and the second medium is a continuous phase, the micro-disperser 6 may be connected to the heavy phase inlet line 1 and then communicated to the tubular reactor 7, and the phase separator 8 is located at the lower end of the tubular reactor.
In this embodiment, the tubular reactor 7 is used to implement a continuous countercurrent absorption or extraction process, where there is no internal structure, which is beneficial for later maintenance and cost savings; the micro-disperser 6 is used for micro-dispersing the dispersed phase and the continuous phase into uniform and controllable micron-sized bubbles or liquid drops, and can adopt a membrane dispersing device or a micro-sieve-hole dispersing device; the phase separator 8, which is used to separate the light phase from the heavy phase, may be an empty pipe separated by a phase interface, or a phase separator containing internals, such as a coalescer.
In the embodiment, uniform and controllable micron-sized bubbles or liquid drops are formed through the micro-disperser 6, the specific surface area is large, and the mass transfer efficiency is high; meanwhile, the size is reduced, so that the ascending or sedimentation rate of the dispersed phase is reduced, the retention time of the dispersed phase is prolonged, the height of equipment is smaller under the same retention time requirement, and the equipment investment and material loss are favorably saved. In addition, the continuous phase and the dispersed phase realize a micro-dispersion process through a circulating pump, and the operation under a large phase ratio (the volume ratio of two phases is more than 10) can be realized.
Preferably, in the case where the first medium is a continuous phase, the second medium is a dispersed phase; alternatively, in the case where the first medium is a dispersed phase, the second medium is a continuous phase.
Wherein the continuous phase refers to a substance in which other substances are dispersed in the dispersion system, and the dispersed phase refers to a substance in which substances are dispersed in the dispersion system.
Preferably, in the case that the first medium is a continuous phase, the second medium is a dispersed phase, and the micro-disperser 6 is connected to the light phase inlet pipe 2 and then communicated with the tubular reactor 7, wherein the lower end of the tubular reactor 7 is further connected to the micro-disperser 6 via a circulation pump for pumping the first medium flowing into the tubular reactor 7 into the micro-disperser 6.
Preferably, the phase separator 8 is located at the upper end of the tubular reactor 7.
Preferably, in the case that the first medium is a dispersed phase, the second medium is a continuous phase, and the micro-disperser 6 is connected to the heavy phase inlet pipeline 1 and then communicated with the tubular reactor 7, wherein the upper end of the tubular reactor 7 is further connected to the micro-disperser 6 via a circulation pump for pumping the second medium flowing into the tubular reactor 7 into the micro-disperser 6.
In another embodiment, the position of the phase separator 8 can also be located at the lower end of the tubular reactor 7.
Preferably, a heavy phase delivery pump is arranged on the heavy phase inlet pipeline 1, and is used for pumping the first medium into the tubular reactor 7; and a light phase delivery pump is arranged on the light phase inlet pipeline 2 and is used for pumping the second medium into the tubular reactor 7.
Preferably, the micro-disperser 6 is a membrane dispersing device or a micro-sieve dispersing device.
Preferably, the micro-sized bubbles or droplets have a size of 50-1000 μm.
Preferably, the volume ratio of the continuous phase to the dispersed phase is from 200:1 to 1: 200.
In this example, the volume ratio of the continuous phase to the dispersed phase is 200:1 to 1:200, and the operation conditions of the macrophase ratio are satisfied.
In particular implementations, the volume ratio of the continuous phase to the dispersed phase can be from 50:1 to 1: 50.
In this embodiment, the ratio of the volume flow rate of the circulation pump to the volume flow rate of the heavy phase transfer pump or the volume flow rate of the light phase transfer pump is 1:5 to 200:1, and when the ratio of the volume flow rate of the circulation pump to the volume flow rate of the heavy phase transfer pump or the volume flow rate of the light phase transfer pump is 1:5 to 200:1, the size of the bubbles or droplets formed by the micro-diffuser is small and uniform.
In specific implementation, the ratio of the volume flow of the circulating pump to the volume flow of the heavy-phase delivery pump or the volume flow of the light-phase delivery pump can be 1:1-50: 1.
Examples 1-5 below take phenol in N-octanol aqueous solution as an example, and examples 6-8 take CO absorption by N-methyldiethanolamine aqueous solution2The present application is illustrated by way of example.
The method for measuring the phenol concentration comprises the following steps: dissolving 0.1g of reaction solution in 4.0g of 1mol/L NaOH solution, analyzing the absorbance of a sample at 280nm by using an ultraviolet-visible spectrophotometer, wherein the reference solution is the 1mol/L NaOH solution, and the calculation formula of the phenol content is shown as the formulas (1) and (2):
A＝εbCm (1)
C＝Cm*a (2)
wherein A is the absorbance, b is the thickness of the sample cell, a is the dilution factor, CmIs the phenol concentration in the sample cell, and C is the phenol concentration. And establishing a standard curve of the absorbance and the phenol concentration by an external standard method, and obtaining the phenol concentration in the actual sample according to the measured absorbance value.
CO2The content is determined by gas chromatography external standard method, CO2The content calculation formula is shown as formula (3):
CCO2＝f*ACO2 (3)
wherein CCO2Is CO2Content, f is a correction factor obtained according to an external standard method, ACO2Is the peak area.
According to the inlet and outlet contents and the flow, the theoretical stage number and the equal plate height can be calculated, and the calculation formula is shown in formulas (4) - (6).
Wherein H is the actual height of the countercurrent column, E is the flow rate of the extract phase or liquid phase, a is the interfacial area of two phases in unit volume, omega is the cross-sectional area of the countercurrent column, KyTotal mass transfer coefficient, y, representing driving force as composition of extract or liquid phase*Is composed of an extract phase or a liquid phase which is in equilibrium with a raffinate phase or a gas phase with the composition x.
Since the solute concentration is low and the two phases are immiscible, E can be regarded as a constant, let K beyAlso approximately constant, equation (4) can be written in the form of equation (5).
Wherein HOEIs the total mass transfer unit height of the dilute solution extract phase or liquid phase, NOEIs the total number of mass transfer units, y, of the dilute solution extract phase or liquid phase0Is the original extractant or solute composition in the liquid phase, yEThe final solute composition in the extract or liquid phase.
Because the relation shown in the formula (6) exists between the theoretical stage number and the total number of the mass transfer units, the theoretical stage number N is usedTAnd equal plate height HeThe calculation is shown in equation (7). In the formula (6), E is the flow rate of an extracting agent or a liquid phase, V is the flow rate of an extracted agent or a gas phase, and m is a two-phase equilibrium relation constant. Wherein the m value of the phenol extraction process is 34, CO2The two-phase equilibrium relationship of the absorption process is shown in Table 1 below.
H＝HeNT (7)
TABLE 1 CO2The temperature of the dissolution equilibrium relation in 2mol/L MDEA water solution is 25 DEG C
Example 1
This example illustrates phenol in an aqueous solution of n-octanol extract solution.
Referring to fig. 2, a schematic structural diagram of an apparatus in which the first medium is a continuous phase in the present application is shown, and as shown in fig. 2, the extraction apparatus includes: a tubular reactor 7, a heavy phase inlet pipeline and a light phase inlet pipeline; the heavy phase inlet pipeline is connected to the upper end of the tubular reactor 7, the light phase inlet pipeline is connected to the lower end of the tubular reactor 7, a heavy phase delivery pump 1 is arranged in the heavy phase inlet pipeline, and a light phase delivery pump 2 is arranged in the light phase inlet pipeline; the micro-disperser 6 is connected with the light phase inlet pipeline and then communicated with the tubular reactor 7, wherein the lower end of the tubular reactor 7 is also connected to the micro-disperser 6 through a circulating pump 5; the upper end of the tubular reactor 7 is also provided with a phase separator 8, wherein the upper end of the phase separator 8 is also communicated with a light phase outlet pump 3, and the lower end of the tubular reactor 7 is also communicated with a heavy phase flow regulating valve 4.
In this example, the tubular reactor 7 had an inner diameter of 10mm and a height of 300 mm; the micro disperser 6 adopts a micro-sieve hole dispersing device; the inner diameter of the phase separator 8 is 15mm, and the height is 50 mm; the heavy phase delivery pump 1, the light phase delivery pump, the light phase outlet pump 3, the heavy phase flow regulating valve 4 and the circulating pump 5 are all common equipment in the field.
The extraction conditions are as follows: 2000ppm of an aqueous phenol solution as a continuous phase and an n-octanol solution as a dispersed phase, wherein the flow rate of the aqueous phenol solution: flow rate of n-octanol solution: the average diameter of the droplets after dispersion by the micro-disperser 6 was 400 μm, with a circulation pump flow rate of 1:0.5: 1.
The extraction process comprises the following steps: the phenol water solution is conveyed to a tubular reactor 7 from a heavy phase inlet A through a heavy phase conveying pump 1 and conveyed to a micro-disperser 6 through a circulating pump 5; the n-octanol solution is delivered from the light phase inlet B to the micro-disperser 6 through the light phase delivery pump 2, and is dispersed with the phenol water solution at the micro-disperser 6 to form uniform controllable micron-sized liquid drops, and then the liquid drops enter the tubular reactor 7 to be subjected to a continuous countercurrent extraction process, and then the liquid drops are subjected to phase separation at the phase separator 8, the light phase is delivered by the light phase outlet pump 3 and flows out of the light phase outlet C, and the heavy phase is delivered by the heavy phase flow regulating valve 4 and flows out of the device through the heavy phase outlet D.
And (3) extraction results: the phenol content of the raffinate is 50ppm, the theoretical stage number is 1.37 and the height of the isobaric plate is 0.22m which can be calculated by the distribution ratio of the phenol in the n-octanol and the water being 34.
Example 2
This example illustrates phenol in an aqueous solution of n-octanol extract solution.
Referring to fig. 2, there is shown a schematic structural view of an apparatus in which the first medium is a continuous phase in the present application, and as shown in fig. 2, the extraction apparatus is the same as in example 1.
Extraction conditions are as follows: flow rate of aqueous phenol solution: flow rate of n-octanol solution: the flow rate of the circulating pump is 100:1:10, and the average diameter of the dispersed liquid drops after passing through the micro-disperser is 300 mu m. The rest is the same as in example 1.
The extraction process comprises the following steps: same as in example 1.
And (3) extraction results: the phenol content of the raffinate is 80ppm, the theoretical stage number is 1.19 and the height of the isobaric plate is 0.25m which can be calculated by the distribution ratio of the phenol in the n-octanol and the water being 34.
Example 3
This example illustrates phenol in an aqueous n-octanol extraction solution.
Referring to fig. 2, there is shown a schematic structural view of an apparatus in which the first medium is a continuous phase in the present application, and as shown in fig. 2, the extraction apparatus is the same as in example 1.
In this example, the height of the tubular reactor 7 was 500mm, and the rest was the same as in example 1.
Extraction conditions are as follows: same as in example 2.
The extraction process comprises the following steps: same as in example 1.
And (3) extraction result: the phenol content of the raffinate is 25ppm, the theoretical stage number is 1.63 and the height of the isobaric plate is 0.31m, which can be calculated from the distribution ratio of phenol in n-octanol and water being 34.
Example 4
This example illustrates phenol in an aqueous solution of n-octanol extract solution.
Referring to fig. 3, a schematic structural diagram of an apparatus in which the first medium is a dispersed phase in the present application is shown, and as shown in fig. 3, the extraction apparatus includes: a tubular reactor 7, a heavy phase inlet pipeline and a light phase inlet pipeline; the heavy phase inlet pipeline is connected to the upper end of the tubular reactor 7, the light phase inlet pipeline is connected to the lower end of the tubular reactor 7, the heavy phase conveying pump 1 is arranged in the heavy phase inlet pipeline, and the light phase conveying pump 2 is arranged in the light phase inlet pipeline; the micro-disperser 6 is connected with the heavy phase inlet pipeline and then communicated with the tubular reactor 7, wherein the upper end of the tubular reactor 7 is also connected to the micro-disperser 6 through a circulating pump 5; the lower end of the tubular reactor 7 is also provided with a phase separator 8, wherein the lower end of the phase separator 8 is also communicated with a light phase outlet pump 3, and the upper end of the tubular reactor 7 is also communicated with a heavy phase flow regulating valve 4.
In this example, the tubular reactor 7 had an inner diameter of 10mm and a height of 300 mm; the micro disperser 6 adopts a micro-sieve hole dispersing device; the inner diameter of the phase separator 8 is 15mm, and the height is 50 mm; the heavy phase delivery pump 1, the light phase delivery pump, the light phase outlet pump 3, the heavy phase flow regulating valve 4 and the circulating pump 5 are all common equipment in the field.
Extraction conditions are as follows: 2000ppm phenol aqueous solution as dispersed phase, n-octanol solution as continuous phase, wherein the flow rate of phenol aqueous solution: flow rate of n-octanol solution: the circulation pump flow rate was 0.5:1:1, and the droplets were dispersed by the micro-disperser 6 and had an average diameter of 600. mu.m.
The extraction process comprises the following steps: the n-octanol solution is conveyed from the light phase inlet B to the tubular reactor 7 through the light phase conveying pump 2 and conveyed to the micro-disperser 6 through the circulating pump 5; the phenol water solution is conveyed to a micro-disperser 6 from a heavy phase inlet A through a heavy phase conveying pump 1, is dispersed with n-octanol solution at the micro-disperser 6 to form uniform and controllable micron-sized liquid drops, then enters a tubular reactor 7 to be subjected to a continuous countercurrent extraction process, and then is subjected to phase separation at a phase separator 8, a light phase is conveyed by a light phase outlet pump 3 to flow out from a light phase outlet C, and a heavy phase is conveyed by a heavy phase flow regulating valve 4 to flow out of the device from a heavy phase outlet D.
And (3) extraction results: the phenol content of the raffinate is 20ppm, and the theoretical stage number is 1.14 and the height of the isobaric plate is 0.26m which can be calculated by the distribution ratio of the phenol in the n-octanol and the water being 34.
Example 5
This example illustrates phenol in an aqueous n-octanol extraction solution.
Referring to fig. 2, there is shown a schematic structural view of an apparatus in which the first medium is a continuous phase in the present application, and as shown in fig. 2, the extraction apparatus is the same as in example 1.
In this example, a membrane dispersion device was used as the micro-diffuser 6, and the rest was the same as in example 1.
Extraction conditions are as follows: the average diameter of the droplets after dispersion by the micro-disperser 6 was 400 μm, and the rest was the same as in example 1.
The extraction process comprises the following steps: same as in example 1.
And (3) extraction result: the phenol content of the raffinate is 60ppm, the theoretical stage number is 1.3 and the height of the isobars is 0.23m according to the calculation result that the distribution ratio of the phenol in the n-octanol to the water is 34.
Example 6
This example uses N-methyldiethanolamine in water to absorb CO2For example.
Referring to fig. 2, which shows a schematic structural view of the device in which the first medium is in a continuous phase in the present application, as shown in fig. 2, the absorption device includes: a tubular reactor 7, a heavy phase inlet pipeline and a light phase inlet pipeline; the heavy phase inlet pipeline is connected to the upper end of the tubular reactor 7, the light phase inlet pipeline is connected to the lower end of the tubular reactor 7, a heavy phase delivery pump 1 is arranged in the heavy phase inlet pipeline, and a light phase delivery pump 2 is arranged in the light phase inlet pipeline; the micro-disperser 6 is connected with the light phase inlet pipeline and then communicated with the tubular reactor 7, wherein the lower end of the tubular reactor 7 is also connected to the micro-disperser 6 through a circulating pump 5; the upper end of the tubular reactor 7 is also provided with a phase separator 8, wherein the upper end of the phase separator 8 is also communicated with a light phase outlet pump 3, and the lower end of the tubular reactor 7 is also communicated with a heavy phase flow regulating valve 4.
In this example, the tubular reactor 7 had an inner diameter of 10mm and a height of 500 mm; the micro-disperser 6 adopts a micro-sieve-hole dispersing device; the inner diameter of the phase separator 8 is 15mm, and the height is 50 mm; the heavy phase delivery pump 1, the light phase delivery pump 2, the light phase outlet pump 3, the heavy phase flow regulating valve 4 and the circulating pump 5 are all common equipment in the field.
Absorption conditions are as follows: 2mol/L N-methyldiethanolamine aqueous solution is used as a continuous phase, and the volume fraction of CO is 1 percent2/N2The mixed gas is used as a dispersion phase and is carried out under the pressure of 0.1MPa and the temperature of 30 ℃. Flow rate of the absorption liquid: gas flow rate: the flow rate of the circulating pump was 1:100:10, and the average diameter of the bubbles after dispersion by the micro-dispenser 6 was 600. mu.m.
And (3) an absorption process: the N-methyldiethanolamine aqueous solution is conveyed from an opening A to a tubular reactor 7 through a heavy phase conveying pump 1, and conveyed to a micro-disperser 6 through a circulating pump 5; CO 22/N2The mixed gas is conveyed to a micro-disperser 6 from a port B through a light phase conveying pump 2, is dispersed with the phenol aqueous solution at the micro-disperser 6 to form uniform and controllable micron-sized bubbles, then enters a tubular reactor 7 to be subjected to a continuous countercurrent absorption process, and then is subjected to phase separation at a phase separator 8, the light phase is conveyed by a light phase outlet pump 3 to flow out from a port C, and the heavy phase is conveyed by a heavy phase flow regulating valve 4 to flow out of the device from a port D.
And (3) absorption results: CO 22Outlet volume fraction 0.05% according to CO2The equilibrium relation with the N-methyldiethanolamine aqueous solution can be calculated to obtain the theoretical stage number of 1.13 and the isoplate height of 0.44 m.
Example 7
This example uses N-methyldiethanolamine in water to absorb CO2For example.
Referring to fig. 2, there is shown a schematic view of the structure of the apparatus in this application in which the first medium is a continuous phase, and as shown in fig. 2, the absorbing apparatus is the same as in example 6.
Absorption conditions are as follows: flow rate of the absorption liquid: gas flow rate: the flow rate of the circulating pump was set to 1:10:10, and the average diameter of bubbles after dispersion by the micro-dispenser 6 was 350 μm, which was otherwise the same as in example 6.
And (3) an absorption process: same as in example 6.
And (3) absorption results: CO 22Outlet volume fraction 0.005% according to CO2With N-methyldiethanolThe equilibrium relation of the amine aqueous solution can be calculated to obtain the theoretical stage number of 1.08 and the height of the isoplate of 0.46 m.
Example 8
This example uses N-methyldiethanolamine in water to absorb CO2For example.
Referring to fig. 2, there is shown a schematic view of the structure of the device in which the first medium is in the continuous phase in the present application, and as shown in fig. 2, the absorbing device is the same as in example 6.
In this example, a membrane dispersion device was used as the micro-diffuser 6, and the rest was the same as in example 6.
Absorption conditions are as follows: the average diameter of the cells after dispersion in the micro-disperser 6 was 400 μm, and the rest was the same as in example 6.
And (3) an absorption process: same as in example 6.
And (3) absorption results: CO 22Outlet volume fraction 0.04% according to CO2The equilibrium relation with the N-methyldiethanolamine aqueous solution can be calculated to obtain the theoretical stage number of 1.21 and the isoplate height of 0.41 m.
The above detailed description is made on a continuous countercurrent device based on a microdispersion technology, and specific examples are applied herein to explain the principle and the implementation of the present application, and the above description of the examples is only used to help understand the method and the core idea of the present application; meanwhile, for a person skilled in the art, according to the idea of the present application, there may be variations in the specific embodiments and the application scope, and in summary, the content of the present specification should not be construed as a limitation to the present application.
Claims (10)
1. A continuous countercurrent device based on microdispersion, comprising: a tubular reactor, a heavy phase inlet pipeline and a light phase inlet pipeline; wherein the heavy phase inlet pipeline is connected to the upper end of the tubular reactor, and the light phase inlet pipeline is connected to the lower end of the tubular reactor;
the tubular reactor is also communicated with a micro-disperser, and the upper end or the lower end of the tubular reactor is also communicated with a phase splitter;
the micro-disperser is used for micro-dispersing a first medium flowing in from the heavy phase inlet pipeline and a second medium flowing in from the light phase inlet pipeline into micron-sized bubbles or liquid drops, the micron-sized bubbles or liquid drops enter the tubular reactor to be subjected to continuous countercurrent absorption or extraction, and then are subjected to phase splitting through the phase splitter to form a light phase and a heavy phase, the light phase flows out through a light phase outlet positioned at the upper end of the tubular reactor, and the heavy phase flows out through a heavy phase outlet positioned at the lower end of the tubular reactor.
2. A continuous countercurrent device based on microdispersion according to claim 1, wherein in case the first medium is a continuous phase, the second medium is a dispersed phase; alternatively, in the case where the first medium is a dispersed phase, the second medium is a continuous phase.
3. The continuous countercurrent device based on the microdispersion technology as claimed in claims 1-2, wherein when the first medium is a continuous phase, the second medium is a dispersed phase, the microdispersion device is connected with the light phase inlet pipeline and then communicated with the tubular reactor, wherein the lower end of the tubular reactor is further connected to the microdispersion device through a circulation pump, and the circulation pump is used for pumping the first medium flowing into the tubular reactor into the microdispersion device.
4. A continuous countercurrent device based on microdispersion technology according to claim 3, characterized in that the position of the phase separator is located at the upper end of the tubular reactor.
5. The continuous countercurrent device based on the microdispersion technology as claimed in claims 1-2, wherein the second medium is a continuous phase when the first medium is a dispersed phase, and the microdispersor is connected to the heavy phase inlet pipe and then communicated with the tubular reactor, wherein the upper end of the tubular reactor is further connected to the microdispersor via a circulation pump, and the circulation pump is used for pumping the second medium flowing into the tubular reactor into the microdispersor.
6. Continuous countercurrent device according to the microdispersion technique, according to claim 5, characterized in that the position of said phase separator is at the lower end of said tubular reactor.
7. The continuous countercurrent device based on the microdispersion technology as claimed in claim 1, wherein a heavy phase delivery pump is arranged on the heavy phase inlet pipeline and is used for pumping the first medium into the tubular reactor; and a light phase conveying pump is arranged on the light phase inlet pipeline and is used for pumping the second medium into the tubular reactor.
8. A continuous countercurrent device based on microdispersion technology according to claim 1, wherein said microdispersion means is a membrane or micromesh dispersion device.
9. A continuous countercurrent device based on microdispersion technology, according to claim 1, characterized in that the micro-bubbles or droplets have a size of 50-1000 μm.
10. The continuous countercurrent device based on the microdispersion technique according to claim 2, characterized in that the volume ratio of said continuous phase to said dispersed phase is from 200:1 to 1: 200.
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| US5160623A (en) * | 1988-10-19 | 1992-11-03 | Stone & Webster Engineering Corp. | Apparatus and process for fluid-fluid contact |
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| JP2014226660A (en) * | 2013-05-17 | 2014-12-08 | 片山 寛武 | Micro counterflow liquid liquid extractor agitating liquid film |
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