CN115569679A - Micro-fluidic chip for rapidly measuring dew point and bubble point - Google Patents
Micro-fluidic chip for rapidly measuring dew point and bubble point Download PDFInfo
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- CN115569679A CN115569679A CN202211473078.6A CN202211473078A CN115569679A CN 115569679 A CN115569679 A CN 115569679A CN 202211473078 A CN202211473078 A CN 202211473078A CN 115569679 A CN115569679 A CN 115569679A
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- 238000006073 displacement reaction Methods 0.000 claims abstract description 32
- 238000004519 manufacturing process Methods 0.000 claims abstract description 14
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- 238000002347 injection Methods 0.000 claims abstract description 5
- 239000007924 injection Substances 0.000 claims abstract description 5
- 238000005530 etching Methods 0.000 claims description 8
- 238000013461 design Methods 0.000 claims description 6
- 239000011148 porous material Substances 0.000 claims description 6
- 238000000605 extraction Methods 0.000 claims description 4
- 238000007789 sealing Methods 0.000 claims description 3
- 230000003321 amplification Effects 0.000 claims description 2
- 238000003199 nucleic acid amplification method Methods 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 6
- 238000011161 development Methods 0.000 abstract description 4
- 238000006243 chemical reaction Methods 0.000 description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 8
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- 229910021641 deionized water Inorganic materials 0.000 description 4
- 230000004069 differentiation Effects 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 229910052594 sapphire Inorganic materials 0.000 description 4
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- 238000000926 separation method Methods 0.000 description 4
- 241001391944 Commicarpus scandens Species 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
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- 238000011160 research Methods 0.000 description 1
- 238000009738 saturating Methods 0.000 description 1
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- B01L3/5027—Containers for the purpose of retaining a material to be analysed, e.g. test tubes with fluid transport, e.g. in multi-compartment structures by integrated microfluidic structures, i.e. dimensions of channels and chambers are such that surface tension forces are important, e.g. lab-on-a-chip
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N25/00—Investigating or analyzing materials by the use of thermal means
- G01N25/56—Investigating or analyzing materials by the use of thermal means by investigating moisture content
- G01N25/66—Investigating or analyzing materials by the use of thermal means by investigating moisture content by investigating dew-point
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/26—Oils; Viscous liquids; Paints; Inks
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Abstract
The invention relates to a micro-fluidic chip for rapidly determining dew point bubble point, which consists of four groups of unit channels, a displacement saturation channel and a production pipeline which are arranged in parallel, wherein the unit channels are arranged in the horizontal direction according to the sequence of amplifying from left to right in equal proportion, and each group of unit channels comprises 5 same channels; each channel is provided with two parts in the vertical direction, namely a top part and a conical part, and the bottom end of the conical part is provided with a capillary tube; the chip is provided with a displacement saturated channel along the horizontal direction, namely the central axis of the unit channel, adjacent unit channels are mutually communicated through the displacement saturated channel, injection ends A1 and A2 are arranged on two sides of the displacement saturated channel, a production end B1 is arranged at the top of the chip, and the top part of the adjacent unit channel is connected with the production end through a production pipeline. The method can accurately measure the black oil bubble point pressure and the condensate gas reservoir dew point pressure, provides an important theoretical basis for evaluating reserves and planning development and production of oil and gas fields, and has great practical significance.
Description
Technical Field
The invention relates to a micro-fluidic chip, in particular to a micro-fluidic chip for rapidly measuring a dew point and a bubble point, and belongs to the technical field of precision detection.
Background
The micro-fluidic technology is a technology for specially researching and processing micro-nano fluid, a micro-fluidic chip can easily construct micro-nano complex flow, and more scholars at home and abroad begin to use the micro-fluidic chip to research the flow and phase change behavior of fluid in the micro-fluidic chip.
Two-phase displacement experiments are mainly carried out by utilizing the micro-fluidic chip, and researchers carry out non-miscible CO by utilizing the micro-fluidic chip 2 Oil displacement and miscible CO 2 Oil displacement and gas-water alternating Oil displacement, and the obtained experimental results were compared with core Experiments (Fuwei, Y. U., et al. Experiments on inhibition mechanisms of fractional reactions by Microfluidic chips. Petroleum extraction and Development 48.5 (2021): 1162-1172), and the student developed three different types of surfactant flooding Experiments with Microfluidic chips (Yu, fuwei, et al. Flow Dynamics of micro-emulsion-formation Surfactants and emulsions for Enhanced Oil Recovery: A fluidic study. SPE International Conference Oil chemistry. EP. 2021). But microfluidic chips for measuring dew point bubble point are not yet available.
The invention designs the micro-fluidic chip for rapidly determining the dew point bubble point, which not only greatly reduces the experimental time, but also can realize the accurate determination of the black oil bubble point pressure and the condensate gas reservoir dew point pressure by only needing a few microliters of samples and changing the position of the micro-fluidic chip, and has important significance for evaluating reserves and planning the development and production of oil and gas fields.
Disclosure of Invention
The invention aims to provide a micro-fluidic chip for rapidly determining a dew point bubble point, which is provided with a micro-nano pore canal, only needs a very small amount of samples and has rapid measurement time, can realize the saturation of high-temperature and high-pressure fluid on the micro-fluidic chip by changing the relation between the pore canal and gravity of the micro-fluidic chip, realizes the accurate determination of a black oil bubble point and a condensate gas dew point, and has wide market application prospect.
In order to achieve the technical purpose, the invention adopts the following technical scheme.
A micro-fluidic chip for rapidly determining dew point bubble point comprises four groups of unit channels, a displacement saturation channel and a production pipeline which are arranged in parallel, wherein the unit channels are arranged in the horizontal direction according to the sequence of amplification from left to right in equal proportion, and each group of unit channels comprises 5 channels with the same size; each channel is provided with two parts in the vertical direction, namely a top part and a conical part, wherein the top part and the conical part are used for accommodating a sample, and the bottom end of the conical part is provided with a capillary tube which is in a sealing design and used for collecting oil drops or bubbles; the chip is provided with a displacement saturated channel along the horizontal direction, namely the central axis of the unit channel, adjacent unit channels are mutually communicated through the displacement saturated channel, injection ends A1 and A2 are arranged on two sides of the displacement saturated channel, the shape and the size of the displacement saturated channel are consistent with those of a fixing hole of a chip clamp, a production end B1 is arranged on the top of the chip, and the top part of the adjacent unit channel is connected with the production end through a production pipeline.
The etching depths of the top part and the conical part of the unit channel are kept consistent, the etching depths of the conical part and the capillary are reduced in a stepped mode, and the volume of the capillary at the lower end of the conical part is designed to be 0.1-0.3% of the total pore volume of the microfluidic chip.
The capillary part of the unit channel is of a sealing design, and oil drops or air bubbles are prevented from escaping.
The design principle of the micro-fluidic chip is designed according to gravity difference and capillary force, and the accurate measurement of the black oil bubble point/condensate gas dew point can be realized by adjusting and rotating the position of the micro-fluidic chip.
Compared with the prior art, the invention has the following beneficial effects:
the microfluidic chip is provided with a micro-nano-scale pore channel, solves the problem of incomplete saturation of the high-temperature and high-pressure fluid microfluidic chip by utilizing the gravity differentiation of fluid, and realizes the identification of liquid drops/bubbles with high resolution by utilizing a special tip under the gravity differentiation. The method can accurately measure the black oil bubble point pressure and the condensate gas reservoir dew point pressure, provides an important theoretical basis for evaluating reserves and planning development and production of oil and gas fields, and has great practical significance.
Drawings
Fig. 1 is a front view of a microfluidic chip for rapidly measuring a bubble point and a dew point.
FIG. 2 is a plan view of a capillary portion at the lower end of a tapered portion of a unit passage.
Fig. 3 is a schematic structural diagram of a microfluidic device for rapidly measuring a bubble point dew point.
In the figure: 1-micro displacement pump; 2-a six-way valve; 3-deionized water intermediate container; 4-an intermediate container; 5-a sample tank; 6-a reaction kettle; 7-sapphire visual window; 8-a microfluidic chip; 9-an electromagnetic heater; 10-a back-pressure valve; 11-a gas-liquid separation tube; 12-a gas flow meter; 13-a back pressure pump; 14-a microscope; 15-an image collector; 16-a light source; 17. 18, 19, 20, 21, 22, 23-valves.
Fig. 4 is a front view of the microfluidic chip when measuring black oil bubble point.
Fig. 5 is a front view of the micro-fluidic chip when measuring the dew point of the condensate gas.
Detailed Description
The invention is further illustrated below with reference to the figures and examples in order to facilitate the understanding of the invention by those skilled in the art. It is to be understood that the invention is not limited in scope to the specific embodiments, but is intended to cover various modifications within the spirit and scope of the invention as defined and defined by the appended claims, as would be apparent to one of ordinary skill in the art.
See fig. 1, 2.
A micro-fluidic chip for rapidly determining dew point bubble points comprises four groups of unit channels which are arranged in parallel, wherein the unit channels are arranged in the horizontal direction according to the sequence of amplifying from left to right in equal proportion, and each group of unit channels comprises 5 channels with the same size; etching 20 channels on a micro-fluidic chip; the axial line position of each unit channel leads all the unit channels to be communicated with the injection ends A1 and A2 at two sides through a channel with the width of 60 micrometers; the top parts of all unit channels are connected with the extraction end B1, and the width of the connected channels is 60 microns.
The unit channel is vertically divided into a top part and a conical part, wherein the width of the top part of the unit channel is designed to be 250 micrometers, 300 micrometers, 350 micrometers and 400 micrometers in sequence, the length of the unit channel is designed to be 5000 micrometers, and the etching depth of the unit channel is 100 micrometers; the width of the tapered part of the unit channel is designed to be 240, 290, 340 and 390 microns, the length is designed to be 1250 microns, and the etching depth is 100 microns; the design can ensure that the top part and the conical part of the microfluidic chip contain a large amount of gas and liquid. The capillary portion at the lower end of the unit channel taper portion was designed to have a width of 10 μm, a length of 100. Mu.m, and an etching depth of 10. Mu.m. The capillary part is designed to be sealed in order to prevent condensed oil droplets/bubbles from escaping and to allow the appearance of condensed oil droplets/bubbles to be detected visually.
See fig. 3.
The micro-fluidic device for rapidly measuring the bubble point dew point comprises a micro displacement pump 1, a deionized water intermediate container 3, an intermediate container 4, a sample tank 5, a reaction kettle 6, a sapphire visible window 7, a micro-fluidic chip 8, an electromagnetic heater 9, a back pressure valve 10, a gas-liquid separation tube 11, a gas flowmeter 12, a back pressure pump 13, a microscope 14, an image collector 15 and a light source 16.
The microfluidic chip 8 is positioned in a reaction kettle 6 with a sapphire visible window 7, the reaction kettle is connected with an electromagnetic heater 9, the inlet end of the reaction kettle is connected with a micro displacement pump 1 through an intermediate container 4 and a sample tank 5, the outlet end of the reaction kettle is connected with a back pressure valve 10, the back pressure valve is respectively connected with a gas-liquid separation tube 11 and a back pressure pump 13, and the gas-liquid separation tube is connected with a gas flowmeter 12; the confining pressure inlet of the reaction kettle is also connected with a trace displacement pump 1 through a deionized water intermediate container 3; a microscope 14 is arranged at the position opposite to the sapphire visual window and is connected with an image collector 15.
See fig. 4.
When the micro-fluidic chip is used for quickly measuring the bubble point, the conical part of the unit channel is vertically upward, and the specific process is as follows:
(1) A1 and A2 of the microfluidic chip 8 are used as displacement saturated inlets, B1 is used as an outlet and is controlled by a back pressure pump, the chip is clamped in the reaction kettle 6, and the position of the microscope 14 is adjusted to enable an image in the image collector 15 to be clearly visible;
(2) Filling the intermediate container 4 with deionized water, filling the sample tank 5 with an oil sample, and checking whether a leak point exists in the whole system;
(3) The micro-fluidic chip 8 is easy to break due to uneven pressure, and simultaneously builds confining pressure and internal pressure, opens the valves 17, 18, 20 and 21, builds the micro-fluidic chip to the experimental pressure at the pump speed of 0.001ml/min through the micro displacement pump 1, continuously applies the back pressure which is 1-2Mpa higher than the internal pressure and the confining pressure through the back pressure pump 13, and simultaneously heats the reaction kettle to the experimental temperature through the electromagnetic heater 9;
(4) Saturating the oil sample, closing valves 18 and 21, opening valves 19 and 22, transferring the oil sample stored in the sample tank 5 into the microfluidic chip through A1 and A2 by using the micro displacement pump 1, wherein the density of the oil sample is lower than that of water, the oil sample floats on the upper layer of the water due to the gravity differentiation, and the water in the microfluidic chip flows out of the chip from the lower part of the microfluidic chip through B1 in the displacement saturation process;
(5) And observing the chip through the image collector 15, judging that sample transfer is finished after water in the chip is completely removed, and closing the back pressure valve 10. And controlling the inlet A2 to continuously reduce the pressure by using the micro displacement pump 1 by taking 0.3MPa as a step length, stabilizing each pressure point for 30min, and indicating that the bubble point of the oil sample is reached when bubbles are observed to be generated in the image collector 15.
See fig. 5.
When the micro-fluidic chip is used for quickly measuring the dew point, the specific process is as follows:
(1) The micro-fluidic chip is turned by 180 degrees clockwise, A1 and A2 of the micro-fluidic chip 8 are used as displacement saturated inlets, and B1 is used as an outlet and is controlled by a back pressure pump. The chip is clamped in the reaction kettle 6, and the position of the microscope 14 is adjusted to ensure that the image in the image collector 15 is clearly visible;
(2) Filling the intermediate container 4 with dry gas, filling the sample tank 5 with condensate gas sample, and checking whether a leakage point exists in the whole system;
(3) Because the micro-fluidic chip 8 is easy to break due to uneven pressure, the ambient pressure and the internal pressure are required to be established together, the valves 17, 18, 20 and 21 are opened, the micro-fluidic chip 8 is established to the experimental pressure at the pump speed of 0.001ml/min through the micro-displacement pump 1, the return pressure which is 1-2Mpa higher than the internal pressure and the ambient pressure is continuously applied through the return pressure pump 13, and the reaction kettle 6 is heated to the experimental temperature by utilizing the electromagnetic heater 9;
(4) The condensate sample is saturated, valves 18 and 21 are closed, and valves 19 and 22 are opened. A condensate gas sample stored in a sample tank 5 is transferred into a microfluidic chip 8 through 10000 times of pore volume of A1 and A2 by using a micro displacement pump 1, the pump speed is 50uL/min, the condensate gas sample density is higher than that of methane, the condensate gas sample is settled at a lower layer due to gravity differentiation, and dry gas in the microfluidic chip 8 can escape from a chip at an extraction channel B1 positioned at the upper part of the microfluidic chip in the displacement saturation process;
(5) The back pressure valve 10 is closed. And controlling the inlet A2 to continuously reduce the pressure by using the micro displacement pump 1 by taking 0.3MPa as a step length, stabilizing each pressure step length for 30min, and when condensate oil droplets are observed to be generated in the image collector 15, indicating that the dew point of the condensate gas sample is reached.
Claims (3)
1. A micro-fluidic chip for rapidly determining dew point bubble points comprises four groups of unit channels, displacement saturation channels and extraction pipelines which are arranged in parallel, and is characterized in that the unit channels are arranged in the horizontal direction according to the sequence of amplification in equal proportion from left to right, and each group of unit channels comprises 5 channels with the same size; each channel is provided with two parts in the vertical direction, namely a top part and a conical part, wherein the top part and the conical part are used for accommodating a sample, and the bottom end of the conical part is provided with a capillary tube which is in a sealing design and used for collecting oil drops or bubbles; the chip is provided with a displacement saturated channel along the horizontal direction, namely the central axis of the unit channel, adjacent unit channels are mutually communicated through the displacement saturated channel, injection ends A1 and A2 are arranged on two sides of the displacement saturated channel, a production end B1 is arranged at the top of the chip, and the top part of the adjacent unit channel is connected with the production end through a production pipeline.
2. The microfluidic chip for rapidly determining the dew point and bubble point of claim 1, wherein the injection ends A1 and A2 disposed at both sides of the displacement saturation channel have the same shape and size as the fixing holes of the chip holder.
3. The microfluidic chip for rapidly determining the dew point and bubble point of claim 1, wherein the etching depth of the top part and the tapered part of the unit channel is kept consistent, the etching depth of the tapered part and the capillary is reduced in a stepwise manner, and the volume of the capillary at the lower end of the tapered part is designed to be 0.1-0.3% of the total pore volume of the microfluidic chip.
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CN115814867A (en) * | 2022-11-23 | 2023-03-21 | 西南石油大学 | Method for rapidly measuring dew point and bubble point by using micro-fluidic chip |
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