CN110455772B - Detection device and analysis method for hydrocarbon concentration of drilling fluid - Google Patents
Detection device and analysis method for hydrocarbon concentration of drilling fluid Download PDFInfo
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- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
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Abstract
The invention discloses a detection device for hydrocarbon concentration of drilling fluid, which applies a Raman spectrometer to detection while drilling, can directly detect hydrocarbon substances in the drilling fluid without gas-liquid separation treatment, has simple integral structure and good timeliness, and can detect the hydrocarbon of upward-returning drilling fluid in real time and rapidly in the drilling process. The invention also provides an analysis method for the hydrocarbon concentration of the drilling fluid, which aims to perform quantitative research on the formula of converting the volume of oil droplets of the oil-containing drilling fluid from the volume below the glass slide to the real volume and the oil droplets in the oil-containing drilling fluid, verify hydrocarbon detection equipment while drilling, obviously detect the Raman spectrum of crude oil in the oil-containing drilling fluid, perform hydrocarbon detection on the drilling fluid in real time in the drilling process, quantitatively identify the concentration of the crude oil in the oil-containing drilling fluid and improve the oil-gas exploration efficiency.
Description
Technical Field
The invention relates to the technical field of petroleum exploration, in particular to a detection device and an analysis method for hydrocarbon-containing concentration of drilling fluid.
Background
In current petroleum exploration, measurement while drilling and logging while drilling technologies are widely applied, and the condition of a stratum close to a drill bit can be reflected more truly through data measured by the measurement while drilling and the logging while drilling. The formation hydrocarbon detection technology in the prior art cannot analyze and detect in real time, the logging hydrocarbon analysis lags behind the well drilling, the quantitative detection of the hydrocarbons is difficult to realize, and the defects often generate analysis results with serious distortion and low quality, so that the analysis results cannot accurately and truly describe reservoir oil and gas information.
The drilling fluid hydrocarbon rapid detection technology based on laser Raman changes the quantitative detection of the formation hydrocarbons from the ground to the underground, can feed back the oil and gas information of the underground reservoir to the ground in real time, provides technical support for more accurately predicting and evaluating the physical property and the productivity of the reservoir, particularly aims at the drilling of directional wells and horizontal wells, can judge whether the running track of a drill bit runs along a preset direction by mastering the underground condition in real time, and ensures the drilling quality. The technology for detecting hydrocarbons from the ground to the underground is a necessary trend in the fields of drilling and logging, and is urgent for real-time and continuous quantitative detection of formation hydrocarbons and detection while drilling. The quantitative detection of the formation hydrocarbons is carried out underground, the safety and the quality of the drilling engineering are improved, meanwhile, the division of layer fineness is facilitated, and technical support is provided for the development of a thin and poor oil layer.
Therefore, it is an urgent need to solve the problem of the art to provide a detection while drilling device and a detection method capable of continuously and quantitatively analyzing the content of liquid hydrocarbons.
Disclosure of Invention
The invention aims to provide a detection device and an analysis method for hydrocarbon concentration of drilling fluid, which are used for solving the problems in the prior art, so that hydrocarbon detection can be carried out on the drilling fluid in real time in the drilling process, and the oil-gas exploration efficiency is improved.
In order to achieve the purpose, the invention provides the following scheme: the invention provides a detection device for hydrocarbon concentration of drilling fluid, which comprises a hollow instrument shell and a pressure-resistant cabin arranged in the instrument shell, wherein the instrument shell can be connected with a drill bit, a closed space is arranged in the pressure-resistant cabin, a Raman spectrometer, a fixer and a quartz optical window are arranged in the pressure-resistant cabin, the Raman spectrometer is provided with a Raman probe, the Raman spectrometer is connected with the Raman probe through an optical fiber, the Raman spectrometer can transmit detection data to external equipment, the Raman probe is arranged on the Raman probe fixer, the quartz optical window is arranged at the bottom of the Raman probe, a sample cell outer tube is arranged at the bottom of the pressure-resistant cabin, the quartz optical window is embedded in the bottom wall of the pressure-resistant cabin and is opposite to the sample cell outer tube, and a drilling fluid return inlet and outlet channel is arranged on the side wall of the instrument shell, the sample cell outer tube is communicated with the external environment through the drilling fluid return access passage, a piston is arranged in the sample cell outer tube, the piston is slidably arranged in the sample cell outer tube, a sealing element is arranged between the piston and the sample cell outer tube, a driver is arranged on one side, away from the drilling fluid return access passage, of the piston, and the driver can drive the piston to move.
Preferably, the bottom of the pressure-resistant cabin is provided with a notch, the notch is provided with an optical window fixer, and the quartz optical window is arranged and connected with the optical window fixer.
Preferably, the raman probe holder is connected with the optical window holder, a sealant is arranged between the raman probe holder and the raman probe, and the raman probe is abutted against the quartz optical window.
Preferably, a filter screen is arranged at the drilling fluid return access passage, and the filter screen can filter rock debris in the drilling fluid.
Preferably, the actuator is a hydraulic cylinder, and the hydraulic cylinder is connected with the piston.
Preferably, a raman spectrometer holder is arranged in the pressure-resistant cabin, the raman spectrometer is arranged on the raman spectrometer holder, and the raman spectrometer is detachably connected with the raman spectrometer holder.
Preferably, a shock absorber is arranged between the raman spectrometer and the raman spectrometer holder, and the shock absorber comprises an elastic member.
The invention also provides an analysis method for the hydrocarbon-containing concentration of the drilling fluid, which comprises the following steps:
step one, after slice observation of the oil-containing drilling fluid, when crude oil accounts for 25% of the oil-containing drilling fluid, when the magnification is 40X, the dispersion degree of oil droplets in the drilling fluid is gradually increased along with the increase of temperature, and when the temperature reaches 65 ℃, the ratio of the oil droplets to the visual field reaches the maximum value;
step two, establishing an identity relation formula by utilizing the principle that the total volume of oil droplets in the drilling fluid and the total volume after flaking is kept unchanged: pi r2h＝4πR3(iii) r is the oil droplet radius in the visual field after flaking, h is flakingThe thickness of the rear oil drop, R is the radius of the oil drop in the drilling fluid; testing the density and weight of the oil-containing drilling fluid, calculating the volume of the oil-containing drilling fluid according to a formula V, wherein rho is the density of the drilling fluid, m is the weight of the oil-containing drilling fluid, and V is the volume of the oil-containing drilling fluidOil-containing drilling fluid＝a2h, wherein a is the side length of the cover sheet, and h is the height of the cover sheet after the sheet is produced and the oil-containing drilling fluid in the glass slide is spread, so that the thickness of the oil-containing drilling fluid under the cover sheet is obtained; the diameter of the oil drop can be counted according to the picture under the mirror, and the counted diameter of the oil drop is substituted into a formula pi r2h＝4πR3In/3, the real volume of the oil droplets can be deduced from the picture under the mirror;
and step three, when the diameter of the oil drop is more than 50 mu m, the oil drop is influenced by interfacial tension, at the moment, two ends of the oil drop do not present a cylindrical shape any more in the flaking process, the interfacial tension of the crude oil at 45-85 ℃ is obtained through calculation, the interfacial tension formula u is substituted into FV rho g/R, wherein u is the interfacial tension, F is the surface tension coefficient, V is the volume of the oil drop, rho is the density of the crude oil, and R is the radius, and the relational expression between the temperature and the volume and the radius of the oil drop is obtained through calculation: 625RT/6468-4325/2156, calculating the diameter of the oil drop according to the picture under the mirror, substituting the calculated diameter of the oil drop into a formula, and deducing the real volume of the oil drop according to the picture under the mirror; when the diameter of the oil drop is smaller than 50 mu m, because the diameter of the oil drop is smaller than the height of the spread oil-containing drilling fluid in the cover slice and the glass slide after the slice making, the oil drop exists in the oil-containing drilling fluid after the slice making in a spherical shape, and the presumed real volume of the oil drop can be presumed by using a sphere formula; when the diameter of the oil droplets is 50 micrometers, the height of the spread oil-containing drilling fluid in the sheet-making cover slice and the glass slide is just reached, the oil droplets are not influenced by interfacial tension, the oil droplets exist in the oil-containing drilling fluid after the sheet-making in a cylindrical form, and the real volume of the oil droplets can be estimated by using a cylindrical formula;
calculating the radius of all oil droplets in the picture according to the picture under the oil-containing drilling fluid with different concentrations, solving the volume of the oil droplets, and establishing a distribution map of the oil droplets in the drilling fluid according to the distribution of the oil droplets at different temperatures;
and step five, obtaining a linear relation between the concentration and the Raman spectrum at 85 ℃ through Raman spectrum analysis of different concentrations: y is 145.8x +1319, wherein x is the crude oil concentration in the oil-containing drilling fluid and y is the raman peak intensity;
step six, the oil-containing drilling fluid is prepared according to the proportion of crude oil with different contents and a certain amount of drilling fluid, the crude oil in the oil-containing drilling fluid is used as a substance to be tested, the drilling fluid can be regarded as a background mixture, and R is madeDrillThe Raman spectrum of the oil-containing drilling fluid R can be obtained according to the spectrum superposition principleMixing ofShould satisfy the spectrum R of the crude oil component to be measuredOilWith the background spectrum RDrillLinear visibility of (a), i.e.:
Rmixing of(v)＝yADrillRDrill(v)+xAOilROil(v) (1-1)
In the formula: a. theDrillRaman intensity of the background mixture, AOilThe Raman intensity of the component to be detected, and v is the wave number;
let KOilThe relative raman intensity coefficient of the mixture of the component to be measured and the background is expressed as:
Koil＝AOil/ADrill (1-2)
Bringing formula (1-2) into formula (1-1):
Rmixing of(v)＝ADrill[yRDrill(v)+xKOilROil(v)] (1-3)
In the formula, x and y are respectively the volume components of crude oil and drilling fluid in the oil-containing drilling fluid, and the volume components can be known
x+y＝1 (1-4)
In order to eliminate the influence of factors such as environment on the Raman spectrum intensity, the measured spectrum of the oil-containing drilling fluid is normalized, and v is madeChinese angelica root-barkAnd (3) expressing the normalized wave number to obtain a normalized spectrum of the oil-containing drilling fluid, wherein the normalized spectrum is as follows:
and then ordering:
the normalized spectrum of the oil-containing drilling fluid can be written as a weighted sum of the drilling fluid and the crude oil to be measured
And seventhly, obtaining a synthesis coefficient of the background spectrum and the spectrum of the component to be detected in the mixture by a spectrum synthesis algorithm, and quantitatively analyzing the concentration of the component to be detected in the mixture to obtain the relationship between the predicted value of the integral quantity of the component to be detected and the relative Raman intensity coefficient and the spectrum synthesis coefficient of the background mixture:
X＝b/(aKoil+b) (1-10)
Wherein
Relative Raman intensity coefficients of a background mixture are shown, and a and b are spectral synthesis coefficients;
step eight, adding crude oil with different volumes into a certain amount of drilling fluid at the temperature of 85 ℃ to obtain four groups of samples, respectively measuring the Raman spectra of the crude oil, the drilling fluid and the oil-containing drilling fluid in the four groups of samples, wherein the integral time of the Raman spectrum of each sample is the same, and measuring for multiple times to obtain an average value; yield 1519cm-1Calculating the average peak value of the drilling fluid and the average value of the crude oil according to the Raman peak value intensity, substituting the results into formulas (1-2), (1-6), (1-7), (1-8) and (1-4) for sequential calculation, and obtaining the calculation result that quantitative analysis can indicate the concentration of the crude oil in the oil-containing drilling fluid;
ninth, analyzing influence factors of quantitative analysis results: in the actual detection process, the temperature is influenced by the depth of the stratum, and the Raman peak intensities of different temperatures at the same wave number rise along with the increase of the temperature, so that the relation between the temperature and the wave number is established:
R(v)T＝3.66T+1595.9 (1-11)
wherein T is temperature, R (v)TThe wave number under the temperature T can be calculated by the formula (1-11) to obtain the Raman spectrum peak intensity of the oil-containing drilling fluid under different temperatures, and the crude oil can be quantitatively analyzed by carrying in the formula after normalization treatment.
Compared with the prior art, the invention has the following technical effects: the detection device for the hydrocarbon concentration of the drilling fluid, disclosed by the invention, applies the Raman spectrometer to detection while drilling, can directly detect hydrocarbon substances in the drilling fluid without gas-liquid separation treatment, has a simple integral structure and good timeliness, and can be used for quickly detecting the hydrocarbons of the upward-returning drilling fluid in real time in the drilling process. The invention also provides an analysis method for the hydrocarbon concentration of the drilling fluid, which aims to perform quantitative research on the formula of converting the volume of oil droplets of the oil-containing drilling fluid from the volume below the glass slide to the real volume and the oil droplets in the oil-containing drilling fluid, verify hydrocarbon detection equipment while drilling, obviously detect the Raman spectrum of crude oil in the oil-containing drilling fluid, perform hydrocarbon detection on the drilling fluid in real time in the drilling process, quantitatively identify the concentration of the crude oil in the oil-containing drilling fluid and improve the oil-gas exploration efficiency.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed to be used in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings without inventive exercise.
FIG. 1 is a device for detecting hydrocarbon concentration of drilling fluid according to the present invention;
FIG. 2 is a spatial distribution diagram of oil globules in an oil-containing drilling fluid containing 75% crude oil in the example;
FIG. 3 is a distribution diagram under a mirror of an oil-containing drilling fluid containing 20% crude oil at different temperatures in the example;
FIG. 4 is the oil droplet area interval under the oil-containing drilling fluid mirror at different temperatures in the example;
FIG. 5 is a comparison of Raman spectra of different substances at 35 ℃ in example;
FIG. 6 shows the Raman shift of 1000cm at different temperatures in the examples-1To 3000cm-1A Raman spectrum peak intensity change diagram under different temperatures;
the device comprises an instrument shell 1, a pressure-resistant cabin 2, a Raman spectrometer 3, a Raman probe fixer 4, a quartz optical window 5, a Raman probe 6, an optical fiber 7, a sample cell outer tube 8, a drilling liquid return access channel 9, a piston 10, a driver 11, an optical window fixer 12, a filter screen 13, a Raman instrument fixer 14, a shock absorber 15 and a drilling liquid channel 16.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention aims to provide a detection device and an analysis method for hydrocarbon concentration of drilling fluid, which are used for solving the problems in the prior art, so that hydrocarbon detection can be carried out on the drilling fluid in real time in the drilling process, and the oil-gas exploration efficiency is improved.
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in further detail below.
Referring to fig. 1-6, wherein fig. 1 is a diagram illustrating the apparatus for detecting the hydrocarbon concentration of the drilling fluid according to the present invention, fig. 2 is a diagram illustrating the spatial distribution of oil droplets in an oil-containing drilling fluid containing 75% crude oil in the example, and fig. 3 is a diagram illustrating an oil-containing drilling fluid containing 20% crude oil in the example at different temperaturesDistribution diagram under the scope of the temperature, FIG. 4 is the area interval of oil droplets under the scope of the oil-containing drilling fluid under different temperatures in the example, FIG. 5 is the comparison diagram of Raman spectra of different substances under 35 ℃ in the example, FIG. 6 is the Raman shift of 1000cm at different temperatures in the example-1To 3000cm-1And (4) a Raman spectrum peak intensity change diagram at different temperatures.
The invention provides a detection device for hydrocarbon concentration of drilling fluid, which comprises a hollow instrument shell 1 and a pressure chamber 2 arranged in the instrument shell 1, wherein the instrument shell 1 can be connected with a drill bit, a closed space is arranged in the pressure chamber 2, a Raman spectrometer 3, a Raman probe fixer 4 and a quartz optical window 5 are arranged in the pressure chamber 2, the Raman spectrometer 3 is provided with a Raman probe 6, the Raman spectrometer 3 is connected with the Raman probe 6 through an optical fiber 7, the Raman spectrometer 3 can transmit detection data to external equipment, the Raman probe 6 is arranged on the Raman probe fixer 4, the quartz optical window 5 is arranged at the bottom of the Raman probe 6, a sample cell outer tube 8 is arranged at the bottom of the pressure chamber 2, the quartz optical window 5 is embedded in the bottom wall of the pressure chamber 2 and is opposite to the sample cell outer tube 8, a drilling fluid return inlet and outlet channel 9 is arranged on the side wall of the instrument shell 1, the sample cell outer tube 8 is communicated with the external environment through the drilling fluid return inlet and outlet channel 9, a piston 10 is arranged in the sample cell outer pipe 8, the piston 10 can be slidably arranged in the sample cell outer pipe 8, a sealing element is arranged between the piston 10 and the sample cell outer pipe 8, a driver 11 is arranged on one side, far away from the drilling return fluid inlet and outlet channel 9, of the piston 10, and the driver 11 can drive the piston 10 to move.
When the device for detecting the hydrocarbon concentration of the drilling fluid is used, after the drill bit drills for a period of time, the drilling fluid returns upwards at the drill bit, the driver 11 drives the piston 10 to move towards the direction far away from the drilling fluid return inlet and outlet channel 9, the drilling fluid is sucked into the sample pool outer tube 8, the Raman spectrometer 3 detects the drilling fluid through the Raman probe 6, after detection is completed, the driver 11 pushes the piston 10 to push out the drilling fluid, the Raman spectrometer 3 transmits detection data to external equipment, the next round of detection can be carried out along with the drilling of the drill bit, the hydrocarbon concentration detection while drilling is realized through the device, and the oil-gas exploration efficiency is improved. Wherein, withstand voltage cabin 2 is airtight cabin, isolated external pressure, can protect the gas in withstand voltage cabin 2, withstand voltage cabin 2 sets up in instrument shell 1, instrument shell 1 sets up the drilling fluid runner, avoid withstand voltage cabin 2 and other settings to influence the normal work of instrument shell 1, raman probe 6 sees through transparent quartz optical window 5 and accomplishes the detection to the drilling fluid, quartz optical window 5 and withstand voltage cabin 2 set up between do sealed processing, set up sealing element between piston 10 and the sample cell outer tube 8, avoid the drilling fluid seepage, can guarantee that piston 10 releases drilling fluid totally after the detection is accomplished simultaneously. In the specific embodiment, the instrument shell 1 is connected with a power source and a data transmitter, the raman spectrometer 3 is connected with a data transmission interface outside the pressure-resistant cabin 2 through a data line, and the data transmission interface is still connected with the data transmitter through the data line to complete data transmission.
In addition, the bottom of the pressure-resistant cabin 2 is provided with a notch, the notch is provided with an optical window fixer 12, the quartz optical window 5 is arranged to be connected with the optical window fixer 12, the optical window fixer 12 is arranged between the pressure-resistant cabin 2 and the quartz optical window 5, the quartz optical window 5 is conveniently connected with the pressure-resistant cabin 2, the processing difficulty of the quartz optical window 5 is reduced, and meanwhile, the air tightness of the pressure-resistant cabin 2 is ensured. The pressure-resistant capacity of the pressure-resistant cabin 2 is more than 150MPa, and the underground operation requirement is met.
Specifically, the Raman probe 6 is arranged on the Raman probe fixing device 4, the Raman probe fixing device 4 is connected with the optical window fixing device 12, sealant is arranged between the Raman probe fixing device 4 and the Raman probe 6 to seal the Raman probe 6 and the external environment, the Raman probe fixing device 4 fixes the position of the probe, the Raman probe 6 is prevented from falling off and dislocating to influence the detection work in the rotation process of the instrument shell 1, the anti-vibration performance of the Raman probe 6 is improved, the Raman probe 6 is abutted to the quartz optical window 5, and the quartz optical window 5 is made of transparent quartz.
More specifically, in order to improve the detection precision, a filter screen 13 is arranged at the drilling fluid return access 9, and the filter screen 13 can filter rock debris in the drilling fluid, so that the influence of mud impurities on the detection of the drilling fluid is avoided. In addition, a drilling fluid channel 16 is further arranged in the instrument shell 1, and the drilling fluid channel 16 is communicated with a drilling fluid circulation channel of the drill rod, so that the drilling of the drill rod is prevented from being influenced.
The driver 11 is a hydraulic cylinder, the hydraulic cylinder is connected with the piston 10, and the hydraulic cylinder can drive the piston 10 to move back and forth. In this embodiment, the driver 11 is a magnetic coupling hydraulic cylinder with an S-pole magnetic push rod inside, the piston 10 has N-pole magnetism, and after the magnetic coupling hydraulic cylinder is powered on, the push rod with S-pole magnetism is pushed by the fracturing oil to move, so as to drive the piston 10 with N-pole magnetism to move. In other embodiments of the present invention, the driver 11 may also be a motor, and the motor drives the piston 10 to move back and forth through a ball screw, and in addition, the present invention is provided with a controller, and the controller is connected with the driver 11, the raman spectrometer 3 and the data transmitter, and the operation of the controller and the controller control device is a conventional means of those skilled in the art, and therefore, the description is omitted.
Further, set up raman appearance fixer 14 in the withstand voltage cabin 2, raman spectrometer 3 sets up on raman appearance fixer 14, and raman appearance fixer 14 provides the installation basis for raman spectrometer 3, and raman spectrometer 3 can be dismantled with raman appearance fixer 14 and be connected, makes things convenient for the dismouting to maintain.
Besides, a shock absorber 15 is arranged between the Raman spectrometer 3 and the Raman spectrometer holder 14, the shock absorber 15 comprises an elastic part, the shock absorber 15 can buffer the shock brought by the instrument shell 1, and the stability of the Raman spectrometer 3 is improved.
The invention also provides an analysis method for the hydrocarbon-containing concentration of the drilling fluid, which comprises the following steps:
step one, after the oil-containing drilling fluid is subjected to sheet observation, when crude oil accounts for 25% of the oil-containing drilling fluid, the dispersion degree of oil droplets in the drilling fluid is gradually increased along with the increase of the temperature when the crude oil accounts for 40X as a magnification factor, the distribution condition of the oil droplets in the drilling fluid is best when the temperature reaches 65 ℃, and the maximum value is reached at the moment through the ratio of the oil droplets to the visual field, which indicates that the crude oil exists in the drilling fluid in the form of large oil droplets.
Step two, establishing an identity relation formula by utilizing the principle that the total volume of oil droplets in the drilling fluid and the total volume after flaking is kept unchanged: pi r2h＝4πR3(iii) r is the oil bead radius in the visual field after flaking; h is the thickness of the oil droplets after tabletting; r isRadius of oil droplets in the drilling fluid. In the experimental process, 2 drops of the drilling fluid are dripped into a glass slide by using a rubber head dropper to prepare the drilling fluid, the weight of two drops of the oil-containing drilling fluid is calculated to be 0.037g through comparison for many times, and the density rho of the prepared drilling fluid is measured to be 1.8g/cm3From the formula: rho is m/v, wherein rho is the density of the drilling fluid; m is the weight of two drops of oil-containing drilling fluid; v is the volume of two drops of oil-containing drilling fluid, and the volume of 2 drops of oil-containing drilling fluid is calculated to be 0.02cm3. From formula VOil-containing drilling fluid＝a2h, a thickness of 50 μm under 2 drops of oil-containing drilling fluid coverslip was obtained. The diameter of the oil drop can be counted according to the picture under the mirror, and the counted diameter of the oil drop is substituted into a formula pi r2h＝4πR3And/3, the true volume of the oil globule can be deduced from the under-the-mirror picture.
And step three, when the diameter of the oil droplets is larger than 50 mu m, the oil droplets are influenced by interfacial tension, at the moment, the two ends of the oil droplets do not present a cylindrical shape any more in the flaking process, the interfacial tension of the Liaohe crude oil is calculated to be 9-24 mN/m at 45-85 ℃, the interfacial tension formula u is substituted into FV rho g/R, wherein u is the Liaohe oil field interfacial tension, F is the surface tension coefficient, 0.22 is selected here, V is the volume of the oil droplets, rho is the density of the crude oil, and R is the radius. And calculating to obtain a relational expression between the temperature and the volume and radius of the oil drop: 625RT/6468-4325/2156, calculating the diameter of the oil drop according to the picture under the mirror, substituting the calculated diameter of the oil drop into a formula, and deriving the real volume of the oil drop according to the picture under the mirror; when the diameter of the oil droplets is less than 50 microns, because the diameter of the oil droplets is less than the height of the spread oil-containing drilling fluid in the sheet-making cover slice and the glass slide, the oil droplets exist in a spherical shape in the oil-containing drilling fluid after the sheet-making, and the estimated actual volume of the oil droplets can be estimated by using a sphere formula; when the diameter of the oil drop is 50 mu m, the oil drop just reaches the height of the spread oil-containing drilling fluid in the cover slice and the glass slide after flaking, and is not influenced by interfacial tension, the oil drop exists in the oil-containing drilling fluid after flaking in a cylindrical form, and the real volume of the oil drop can be estimated by using a cylindrical formula.
And step four, calculating the radius of all oil droplets in the image according to the pictures under the oil-containing drilling fluid lens with different concentrations, so as to calculate the volume of the oil droplets, and establishing a distribution map of the oil droplets in the drilling fluid according to the distribution of the oil droplets at different temperatures, as shown in figure 2.
And step five, obtaining a linear relation between the concentration and the Raman spectrum at 85 ℃ through Raman spectrum analysis of different concentrations: and y is 145.8x +1319, wherein x is the crude oil concentration in the oil-containing drilling fluid, and y is the Raman peak intensity.
Step six, the oil-containing drilling fluid is prepared according to the proportion of crude oil with different contents and a certain amount of drilling fluid, the crude oil in the oil-containing drilling fluid is used as a substance to be tested, the drilling fluid can be regarded as a background mixture, and R is madeDrillRaman spectra of the background mixture are shown. The Raman spectrum R of the oil-containing drilling fluid can be obtained according to the spectrum superposition principleMixing ofThe linear visibility of the crude oil composition spectrum R oil to be measured and the background spectrum R drill should be satisfied, namely:
Rmixing of(v)＝yADrillRDrill(v)+xAOilROil(v) (1-1)
In the formula: a. theDrillRaman intensity of the background mixture, AOilThe Raman intensity of the component to be measured is shown, and v is the wave number.
Let KOilThe relative raman intensity coefficient of the mixture of the component to be measured and the background is expressed as:
Koil＝AOil/ADrill (1-2)
Bringing formula (1-2) into formula (1-1):
Rmixing of(v)＝ADrill[yRDrill(v)+xKOilROil(v)] (1-3)
In the formula, x and y are respectively the volume components of crude oil and drilling fluid in the oil-containing drilling fluid, and the volume components can be known
x+y＝1 (1-4)
In order to eliminate the influence of factors such as environment on the Raman spectrum intensity, the measured spectrum of the oil-containing drilling fluid is normalized to ensure that v isChinese angelica root-barkAnd (3) expressing the normalized wave number to obtain a normalized spectrum of the oil-containing drilling fluid, wherein the normalized spectrum is as follows:
and then ordering:
the normalized spectrum of the oil-containing drilling fluid can be written as a weighted sum of the drilling fluid and the crude oil to be measured
Seventhly, using oil-containing drilling fluid containing 33 percent of crude oil at 75 ℃ to reach 1519cm-1The peak value is taken as an example, the vibration displacement of the oil drilling fluid is 1519cm-1The peak at this time is 1724; the peak value of the drilling fluid under the displacement is 1067; the peak value of the crude oil at this displacement was 1200. Substituting the equations (1-2) - (1-8) to calculate, and normalizing the wave number at the moment to obtain the relation equation containing the drilling fluid at the moment:
step eight, if the synthesis coefficients of the background spectrum and the spectrum of the component to be detected in the mixture are obtained by the spectrum synthesis algorithm, and the concentration of the component to be detected in the mixture is quantitatively analyzed, the relationship between the predicted value of the integral quantity of the component to be detected and the relative Raman intensity coefficient and the spectrum synthesis coefficient of the background mixture is obtained:
X＝b/(aKoil+b) (1-10)
Wherein the content of the first and second substances,
relative Raman intensity coefficients of background mixture, a and bSpectral composition coefficient.
Step nine, adding crude oil with different volumes into 40ml of drilling fluid at the temperature of 85 ℃ to obtain four groups of samples, respectively measuring the Raman spectra of the crude oil, the drilling fluid and the oil-containing drilling fluid in the four groups of samples, wherein the integral time of the Raman spectrum of each sample is 3s, and measuring for multiple times to obtain an average value to obtain 1519cm-1The Raman peak value is 1521, the average peak value of the drilling fluid is 1247, the average score of the crude oil is 1127, the Raman peak value and the average score are substituted into the formulas (1-2) (1-6) (1-7) (1-8) (1-4) to be calculated in sequence, and the calculation results are shown in the table 1. As can be seen from Table 1, the calculation error gradually increases with the increase of the crude oil concentration, but the error does not exceed 1% in general, thereby indicating that the quantitative analysis can well indicate the concentration of the crude oil in the oil-containing drilling fluid.
Comparing the real value and the calculated value of the oil-containing drilling fluid with different concentrations at 185 ℃ in the table
Tenthly, analyzing influence factors of the quantitative analysis result: in the actual detection process, the temperature is influenced by the depth of the stratum, and the Raman peak intensities of different temperatures at the same wave number rise along with the increase of the temperature, so that the relation between the temperature and the wave number is established:
R(v)T＝3.66T+1595.9 (1-11)
wherein T is temperature, R (v)TThe wave number at temperature T. The Raman spectrum peak intensity of the oil-containing drilling fluid at different temperatures can be deduced by the formula (1-11), and the crude oil can be quantitatively analyzed by carrying out normalization treatment and then substituting the normalized Raman spectrum peak intensity into the formula.
The method for analyzing the hydrocarbon concentration of the drilling fluid simulates the Raman spectrum research of the oil-containing drilling fluid with different oil contents in the well under the condition of normal pressure under the condition of gradually rising temperature, the distribution state of the crude oil in the drilling fluid and the condition of being influenced by the temperature, and the distribution condition research of the crude oil under different concentrations in the drilling fluid, and utilizes the laser Raman technology to rapidly detect the hydrocarbon substances in the oil-containing drilling fluid to obtain the Raman spectrum which is compared with the Raman spectrum of the crude oil. In the spectral analysis of hydrocarbons, the characterizing parameters of the spectral characteristics of hydrocarbons are mainly spectral shifts and intensities. The Raman spectrogram can be directly read, if the noise influence of the Raman spectrogram is large, the spectrum is processed by means of fluorescence filtering, data smoothing, wavelet transformation, derivative filtering and the like to obtain the clear Raman spectrogram with obvious hydrocarbon Raman characteristics, and a mathematical model is established by combining a regression method of linear correlation, polynomial relation and exponential relation. The invention can verify hydrocarbon detection equipment while drilling through tests, can obviously detect the Raman spectrum of the crude oil in the oil-containing drilling fluid, can detect the hydrocarbon of the drilling fluid in real time in the drilling process, can identify each component in the crude oil, lays a solid foundation for theoretical analysis to actual application of hydrocarbon detection while drilling, real time and the like, and can obtain the oil-containing drilling fluid weight sum formula after normalization by quantitatively identifying the crude oil in the oil-containing drilling fluid.
The principle and the implementation mode of the invention are explained by applying a specific example, and the description of the embodiment is only used for helping to understand the method and the core idea of the invention; meanwhile, for a person skilled in the art, according to the idea of the present invention, the specific embodiments and the application range may be changed. In view of the above, the present disclosure should not be construed as limiting the invention.
Claims (5)
1. A method for analyzing the hydrocarbon concentration of drilling fluid is based on a detection device of the hydrocarbon concentration of the drilling fluid, the detection device comprises a hollow instrument shell and a pressure-resistant cabin arranged in the instrument shell, the instrument shell can be connected with a drill bit, a closed space is arranged in the pressure-resistant cabin, a Raman spectrometer, a Raman probe fixer and a quartz optical window are arranged in the pressure-resistant cabin, the Raman spectrometer is provided with a Raman probe, the Raman spectrometer is connected with the Raman probe through an optical fiber, the Raman spectrometer can transmit detection data to external equipment, the Raman probe is arranged on the Raman probe fixer, the quartz optical window is arranged at the bottom of the Raman probe, a sample cell outer tube is arranged at the bottom of the pressure-resistant cabin, and the quartz optical window is embedded in the bottom wall of the pressure-resistant cabin and is opposite to the sample cell outer tube, a drilling fluid return access passage is arranged on the side wall of the instrument shell, the sample cell outer tube is communicated with the external environment through the drilling fluid return access passage, a piston is arranged in the sample cell outer tube, the piston is slidably arranged in the sample cell outer tube, a sealing element is arranged between the piston and the sample cell outer tube, a driver is arranged on one side of the piston, which is far away from the drilling fluid return access passage, and the driver can drive the piston to move; a notch is formed in the bottom of the pressure-resistant cabin, an optical window fixer is arranged at the notch, and the quartz optical window is connected with the optical window fixer; the Raman probe fixing device is connected with the optical window fixing device, a sealant is arranged between the Raman probe fixing device and the Raman probe, and the Raman probe is abutted against the quartz optical window;
the method for analyzing the hydrocarbon concentration of the drilling fluid is characterized by comprising the following steps of:
step one, after slice observation of the oil-containing drilling fluid, when crude oil accounts for 25% of the oil-containing drilling fluid, when the magnification is 40X, the dispersion degree of oil droplets in the drilling fluid is gradually increased along with the increase of temperature, and when the temperature reaches 65 ℃, the ratio of the oil droplets to the visual field reaches the maximum value;
step two, establishing an identity relation formula by utilizing the principle that the total volume of oil droplets in the drilling fluid and the total volume after flaking is kept unchanged: pi r2h＝4πR3In the formula, R is the radius of the oil drop in the visual field after flaking, h is the thickness of the oil drop after flaking, and R is the radius of the oil drop in the drilling fluid; the density and weight of the oil-containing drilling fluid are tested, the volume of the oil-containing drilling fluid is calculated according to a formula p ═ m/v, wherein p is the density of the oil-containing drilling fluid, m is the weight of the oil-containing drilling fluid, v is the volume of the oil-containing drilling fluid, and then the formula v ═ a2h, wherein a is the side length of the cover glass, and h is the height of the spread cover glass after the slide is sliced and the oil-containing drilling fluid in the slide glass, so as to obtain the thickness of the oil-containing drilling fluid under the cover glass; the diameter of the oil drop can be counted according to the picture under the mirror, and the diameter of the oil drop is calculated according to the picture under the mirrorSubstituting the counted diameter of the oil drop into a formula pi r2h＝4πR3In/3, the real volume of the oil droplets can be deduced from the picture under the mirror;
and step three, when the diameter of the oil drop is more than 50 mu m, the oil drop is influenced by interfacial tension, at the moment, two ends of the oil drop do not present a cylindrical shape any more in the flaking process, the interfacial tension of the crude oil at 45-85 ℃ is obtained through calculation, the interfacial tension formula u is substituted into FV rho g/R, wherein u is the interfacial tension, F is the surface tension coefficient, V is the volume of the oil drop, rho is the density of the crude oil, and R is the radius, and the relational expression between the temperature and the volume and the radius of the oil drop is obtained through calculation: 625RT/6468-4325/2156, calculating the diameter of the oil drop according to the picture under the mirror, substituting the calculated diameter of the oil drop into a formula, and deriving the real volume of the oil drop according to the picture under the mirror; when the diameter of the oil drop is smaller than 50 mu m, because the diameter of the oil drop is smaller than the height of the spread oil-containing drilling fluid in the cover glass and the glass slide after the slide is made into a sheet, the oil drop exists in the oil-containing drilling fluid after the sheet is made into a spherical shape, and the presumed true volume of the oil drop can be presumed by using a sphere formula; when the diameter of the oil droplets is 50 micrometers, the oil droplets just reach the height of the spread oil-containing drilling fluid in the cover glass and the glass slide after the slide is sliced, and are not influenced by interfacial tension, the oil droplets exist in the oil-containing drilling fluid after the slide is sliced in a cylindrical form, and the real volume of the oil droplets can be estimated by using a cylindrical formula;
calculating the radius of all oil droplets in the picture according to the picture under the oil-containing drilling fluid with different concentrations, solving the volume of the oil droplets, and establishing a distribution map of the oil droplets in the drilling fluid according to the distribution of the oil droplets at different temperatures;
and step five, obtaining a linear relation between the concentration and the Raman spectrum at 85 ℃ through Raman spectrum analysis of different concentrations: y is 145.8x +1319, wherein x is the crude oil concentration in the oil-containing drilling fluid and y is the raman peak intensity;
step six, the oil-containing drilling fluid is prepared according to the proportion of crude oil with different contents and a certain amount of drilling fluid, the crude oil in the oil-containing drilling fluid is used as a substance to be tested, the drilling fluid is regarded as a background mixture, and R is madeDrillRaman spectra representing background mixtures, according to lightThe Raman spectrum R of the oil-containing drilling fluid can be obtained by the spectrum superposition principleMixing ofShould satisfy the spectrum R of the crude oil component to be measuredOilWith the background spectrum RDrillLinear visibility of (a), i.e.:
Rmixing of(v)＝yADrillRDrill(v)+xAOilROil(v) (1-1)
In the formula: a. theDrillRaman intensity of the background mixture, AOilThe Raman intensity of the component to be detected, and v is the wave number;
let KOilThe relative raman intensity coefficient of the mixture of the component to be measured and the background is expressed as:
Koil＝AOil/ADrill (1-2)
Substituting formula (1-2) into formula (1-1):
Rmixing of(v)＝ADrill[yRDrill(v)+xKOilROil(v)] (1-3)
In the formula, x and y are respectively the volume components of crude oil and drilling fluid in the oil-containing drilling fluid, and the volume components can be known
x+y＝1 (1-4)
In order to eliminate the influence of environmental factors on the Raman spectrum intensity, the measured spectrum of the oil-containing drilling fluid is normalized, and v is madeChinese angelica root-barkAnd (3) expressing the normalized wave number to obtain a normalized spectrum of the oil-containing drilling fluid, wherein the normalized spectrum is as follows:
and then ordering:
the normalized spectrum of the oil-containing drilling fluid can be written as a weighted sum of the drilling fluid and the crude oil to be measured
And seventhly, obtaining a synthesis coefficient of the background spectrum and the spectrum of the component to be detected in the mixture by a spectrum synthesis algorithm, and quantitatively analyzing the concentration of the component to be detected in the mixture to obtain the relationship between the predicted value of the integral quantity of the component to be detected and the relative Raman intensity coefficient and the spectrum synthesis coefficient of the background mixture:
X＝b/(aKoil+b) (1-10)
Wherein
Relative Raman intensity coefficients of a background mixture are shown, and a and b are spectral synthesis coefficients;
step eight, adding crude oil with different volumes into a certain amount of drilling fluid at the temperature of 85 ℃ to obtain four groups of samples, respectively measuring the Raman spectra of the crude oil, the drilling fluid and the oil-containing drilling fluid in the four groups of samples, wherein the integral time of the Raman spectrum of each sample is the same, and measuring for multiple times to obtain an average value; yield 1519cm-1Calculating the average peak value of the drilling fluid and the average value of the crude oil by using the Raman peak value intensity, substituting the results into formulas (1-2), (1-6), (1-7), (1-8) and (1-4) to calculate in sequence, and obtaining the calculation result, wherein the quantitative analysis can explain the concentration of the crude oil in the oil-containing drilling fluid;
ninth, analyzing influence factors of quantitative analysis results: in the actual detection process, the temperature is influenced by the depth of the stratum, and the Raman peak intensities of different temperatures at the same wave number rise along with the increase of the temperature, so that the relation between the temperature and the wave number is established:
R(v)T＝3.66T+1595.9 (1-11)
wherein T is temperature, R (v)TThe wave number under the temperature T can be calculated by the formula (1-11), the Raman spectrum peak intensity of the oil-containing drilling fluid under different temperatures can be calculated, and the crude oil can be quantitatively analyzed by substituting the normalized wave number into the formula.
2. The method for analyzing the hydrocarbon-containing concentration of drilling fluid according to claim 1, wherein: and a filter screen is arranged at the drilling fluid return access passage and can filter rock debris in the drilling fluid.
3. The method for analyzing the hydrocarbon-containing concentration of drilling fluid according to claim 1, wherein: the driver is a hydraulic cylinder, and the hydraulic cylinder is connected with the piston.
4. The method for analyzing the hydrocarbon-containing concentration of drilling fluid according to claim 1, wherein: the pressure-resistant cabin is internally provided with a Raman instrument fixer, the Raman spectrometer is arranged on the Raman instrument fixer, and the Raman spectrometer is detachably connected with the Raman instrument fixer.
5. The method for analyzing the hydrocarbon-containing concentration of drilling fluid according to claim 4, wherein: a shock absorber is arranged between the Raman spectrometer and the Raman spectrometer holder and comprises an elastic piece.
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