CN106053166A - Crude oil emulsion preparation method based on apparent viscosity quantitative characterization - Google Patents
Crude oil emulsion preparation method based on apparent viscosity quantitative characterization Download PDFInfo
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Abstract
The invention relates to a crude oil emulsion preparation method based on apparent viscosity quantitative characterization. The preparation method comprises the following steps: at first, obtaining the crude oil accumulated precipitated wax amounts at different temperatures that are below the wax precipitation temperature; determining the density of crude oil emulsion preparation temperature; taking out a crude oil sample from an oil barrel, filling the crude oil sample into multiple sealed bottles with a ground stopper, carrying out a pretreatment; measuring the crude oil solidification point and balanced apparent viscosity; preparing crude oil emulsion that is used to obtain the quantitative characterization parameters of apparent viscosity; measuring the apparent viscosity of prepared crude oil emulsion, calculating the viscosity flowing entropy production value under each preparation condition; and accurately choosing stirring conditions for preparing emulsion according to known physical properties such as blank crude oil density, apparent viscosity, and wax precipitation characteristics, and the like. The preparation method is used to produce mimic crude oil emulsion, which has the rheological properties that is similar with crude oil under practical production conditions, and thus a foundation is provided for the research on rheological properties of crude oil emulsion.
Description
Technical field
The present invention relates to the preparation technique of the crude oil emulsion that experimentation is used, be based particularly on apparent viscosity and quantify
The crude oil emulsion compound method characterized.
Background technology
Along with oil development develops to deep-sea, mixed transportation of oil and gas is by main for the offshore oilfield gathering line becoming relatively long distance
One of mode of movement.In oil mixing with water course of conveying, at well head, pump and choke valve etc., oil-water mixture can stand height
Speed is sheared, and forms crude oil emulsion.The rheological characteristic of crude oil emulsion is the main foundation data of Oil-water Mixed Transmission Pipelines design management
One of, also it is the final determiner that can restart safely of crude water blending transportation pipeline, is that pipeline shutdown restarts calculating
The important foundation data evaluated with pumpability.
The measurement of crude oil emulsion rheological behavior typically completes at laboratory, the most of crude oil including waxy crude oil
Emulsion, when the test specimen of production scene sampling is until measuring, owing to experienced by prolonging of shear history, thermal history and time
Continuous, the problem such as rheological equationm of state change and flocculation breakdown of emulsion occurs.Therefore, most researcher uses laboratory preparation fresh crude oil emulsus
Liquid is laboratory sample.How preparing the simulating oil-water emulsion identical with the rheological equationm of state under actual production conditions is measurement Research
Basis.
Crude oil emulsion has all rheological characteristic features of crude oil, and formed condition has the strongest according to lazyness.
The measurement of existing Laboratory Crude Oil emulsion rheological behavior is according to moisture content, (includes stirring under a certain specific preparation condition
Mix speed, mixing time, add water mode etc.) laboratory sample that formed, causing measurement result is also under this preparation condition
Data, the emulsifying degree of laboratory sample whether with produce that reality is identical cannot probe into, therefore measurement result is applied to actual life
Product produces very large deviation.Apparent viscosity is one of main characterization parameter of crude oil emulsion emulsifying degree rheological behavior, therefore
Carry out crude oil emulsion compound method research based on apparent viscosity quantization signifying.
Summary of the invention
It is an object of the invention to provide crude oil emulsion compound method based on apparent viscosity quantization signifying, this based on table
The crude oil emulsion compound method seeing viscosity quantization signifying is real with production for the crude oil emulsion solving the preparation of existing laboratory
The problem that emulsifying degree in border cannot quantitatively not correspond.
The technical solution adopted for the present invention to solve the technical problems is: this crude oil based on apparent viscosity quantization signifying
Emulsion compound method is as follows:
Step one: 4 ~ 8 mg will be weighed from oil drum after production scene takes crude oil sample to be placed in and transport to laboratory oil drum
Crude oil sample insert in aluminum cup seal, the crucible after sealing is put in the measuring cell of differential calorimetric scan instrument, is heated to
80 DEG C and constant temperature 1min, then it is cooled to-20 DEG C from 80 DEG C in a nitrogen atmosphere, in conjunction with thermography with the rate of temperature fall of 5 DEG C/min
Figure curve, is defined as the temperature beginning to deviate from baseline the wax precipitation point of crude oil；It is calculated the following temperature of wax precipitation temperature again
Crude oil accumulation analysis wax amountc w；
Step 2: again measure crude oil sample from oil drum, is heated to oil sample mobility preferably certain temperature, measures dehydration
The standard density of crude oil, then the density of crude oil emulsion preparation temperature is determined by the standard density of crude oil；
Step 3: taking out crude oil sample again from oil drum and be dispensed into several and seal in port grinding bottles and carry out pretreatment, will should
The sealing port grinding bottle batch filling crude oil sample is put in water-bath simultaneously, stands and is heated to 80 DEG C and constant temperature 2h, takes out above-mentioned sealing
Port grinding bottle stands and naturally cools to room temperature, deposits in variation of ambient temperature smaller part standing more than 48h standby；
Step 4: arbitrarily take out one from step 3 pretreated crude oil sample and seal port grinding bottle, according to petroleum gas
Industry standard SY/T 0541-2009 " condensation point of crude oil algoscopy ", uses petroleum products questionable points instrument to measure condensation point of crude oil；
Step 5: further take out several from step 3 pretreated crude oil sample and seal port grinding bottle, according to petroleum gas
Industry standard SY/T 0520-93 " viscosity of crude mensuration-rotating cylinder viscometer counterbalanced procedure ", uses viscometer to measure crude oil in condensation point
Balance apparent viscosity at neighbouring temperature；
Step 6: be formulated for obtain apparent viscosity quantitatively characterizing parameter use crude oil emulsion, crude oil sample used be through
Step 3 is pretreated, take wherein one bottle put into water-bath airtight be heated to prepare temperature, constant temperature 30 min；By volume moisture contentn w, oil density, water densityMeasure the quality of continuous phase and dispersion phase respectively, continuous phase and dispersion phase have been fallen simultaneously
Entering preheated dosing beaker, and use digital display agitator to stir, stirring paddle is placed in beaker central authorities bottom 5mm at the bottom of at the bottom of cup,
Stir sometime under a certain stir speed (S.S.), form the crude oil emulsion needed, prepare the crude oil of basic, normal, high 3 moisture content
Emulsion, each moisture content crude oil emulsion respectively in basic, normal, high 3 shear rates, basic, normal, high 3 shear times, 9 kinds
Formed under preparation condition；
Step 7: determination step six prepares the apparent viscosity of crude oil emulsion, a certain moisture content that step 6 prepares, preparation
Under the conditions of crude oil emulsion carry out crude oil emulsion apparent viscosity mensuration according to the apparent viscosity measuring method of step 5；Preparation
After good fresh emulsion loads rheometry cylinder according to measurement standard, residue emulsion is filled to rapidly emulsion stability
Observe in test tube, and be placed in the program control water-bath of flow graph, make the emulsion in observation test tube and laboratory sample in flow graph
Experience identical thermal history, to observe in flow graph sample whether breakdown of emulsion；
Measure the apparent viscosity of crude oil emulsion at two temperature: one is preparation temperature, and two is temperature to be characterized；
At a temperature of crude oil emulsion is prepared, owing to, more than wax precipitation point temperature, crude oil normally behaves as Newtonian fluid characteristic, low
Moisture content crude oil emulsion also shows as Newtonian fluid characteristic, need to survey balance apparent viscosity；And the emulsion of middle high-moisture percentage
Showing as non-Newton fluid characteristic, meet power-law fluid constitutive relation, its constitutive equation is as follows, according to apparent viscosity data, intends
Close out crude oil emulsionK 、nValue；
In formulaFor shear stress, Pa；
For shear rate, s-1;
kFor consistency coefficient, Pa sn；
N is rheological behavior index, immeasurable firm amount；
Step 8: according to the condition of step 6 preparation emulsion, calculate the VISCOUS FLOW entropy output value under each preparation condition, suitable
For calculating the expression formula of the low-water-content Newtonian fluid speciality crude emulsion VISCOUS FLOW entropy output value it is:
Be applicable to calculating, the expression formula of the high-moisture percentage non-Newton fluid characteristic crude oil emulsion VISCOUS FLOW entropy output value is:
In this step two formulaThe volumetric water content of emulsion, %；
、It is respectively water and the density of crude oil, kg/m3；
TThe actual control temperature of agitator tank, i.e. whipping temp, K；
Speed of agitator, r/s；
Metzner constant, takes estimated value 11；
The viscosity of Newtonian fluid, Pa s；
Consistency coefficient in power law model, or power law coefficient, Pa sn；
Liquidity index in power law model, or referred to as power law index, dimensionless；
Mixing time, s；
Emulsion is preparedVISCOUS FLOW entropy in time period produces, J/kg K；
Step 9: the VISCOUS FLOW entropy output value of crude oil emulsion process for preparations g, crude oil analysis wax amount at temperature to be characterizedc w,
Blank crude oil apparent viscosity, the apparent viscosity of crude oil emulsionAnd the shear rate that apparent viscosity measures5 parameters
Meet following relation
In formulaa 0 、a 1 、a 2 、a 3 、a 4Fitting parameter；
By the VISCOUS FLOW entropy output value of each process for preparations g, blank crude oil apparent viscosity, a certain temperature crude oil analysis
Wax amountc w, measure emulsion apparent viscosity time shear rateLogarithm value as the basic data of independent variable, will not
With the emulsion balance apparent viscosity that process for preparation is correspondingLogarithm value as the basic data of dependent variable, to following expression
Formula, utilizes method of least square to carry out linear fit；
Obtain fitting parametera 0 、a 1 、a 2 、a 3 、a 4Value, then above formula is carried out indexation, obtains following expression:
I.e.
This formula is applicable to cattle
Pause fluid；
This formula is applicable to non-
Newtonian fluid；
In formulaShear rate, s-1；
Blank viscosity of crude, mpa s；
Crude oil analyses wax amount, % in a certain temperature；
Step 10: under the physical property premises such as known blank oil density, apparent viscosity, analysis wax characteristic, be intended to prepare given moisture content,
The Simulation of Crude Oil emulsion of a certain apparent viscosity at a temperature of determining, according to above-mentioned expression formula, when accurately selecting preparation emulsion
Stirring condition, i.e. according to formulated in combination crude oil based on the apparent viscosity quantization signifying emulsus of different mixing speeds with mixing time
Liquid.
In such scheme step one: according to oil and gas industry standard SY/T 0545-2012 " crude oil analysis wax thermal characteristics
The determination of parameter: differential scanning calorimetry ", use modulation system differential scanning calorimeter to measure the analysis wax characteristic of crude oil, specifically side
Method is: sealing in aluminum cup inserted by the crude oil sample weighing 4 ~ 8 mg, and differential calorimetric scan instrument put into by the crucible after sealing
In measuring cell, it is heated to 80 DEG C and constant temperature 1min, then with the rate of temperature fall of 5 DEG C/min at the nitrogen that flow velocity is 50 ml/min
It is cooled to-20 DEG C from 80 DEG C under atmosphere, in conjunction with Thermogram DSC curve, the temperature beginning to deviate from baseline is defined as the analysis of crude oil
Wax point WAT；With the area integral of composition between heat flow curve and the baseline of temperature range a certain on curve, divided by the average knot of wax
Brilliant heat content, obtains the crude oil accumulation analysis wax amount of the following temperature of wax precipitation temperaturec w, available following formula calculates:
In formula,The concentration brilliant for separating out wax, wt%；For to measure the temperature of analysis wax amount, DEG C；dQFor temperature fromT +dT
It is down toTTime analysis wax crystallization thermal discharge, J/g；For the average crystallite heat content of wax, depend on the composition of wax, typically take 210J/
g。
Such scheme step 2 determines the density of crude oil emulsion preparation temperatureMethod:
(1) according to taken former oil properties, oil sample is heated to the preferable temperature of mobility, such as 50 DEG C；
(2) the crude oil sample of a certain temperature (such as 50 DEG C) will be risen to, pour in density measure cylinder along inwall carefully, density measure
Cylinder is placed in design temperature (such as 50 DEG C) waters groove, and thermometer is placed in density measure cylinder in oil sample；
(3) densimeter is put in crude oil sample to be measured, after the free floating stable of densimeter, read densimeter and temperature simultaneously
The measurement result of meter；
(4) record the oil sample density of double mensuration, average as this temperature (owing to there being heat to dissipate during measuring
Lose, temperature is as the criterion with temperature reading) under crude oil sample density, and according to following formula calculate crude oil standard density,
Obtain the standard density of crude oilAfter, crude oil emulsion preparation temperature (such as 45 DEG C) can be determined by above-mentioned expression formula
Time density
According to oil and gas industry standard SY/T 0541-2009 " condensation point of crude oil algoscopy " in such scheme step 4, use
Petroleum products questionable points instrument measures condensation point of crude oil, and method is: after filling sample temperature dress sample more than crude oil wax precipitation point, with 0.5～1.0
DEG C/the rate of temperature fall cooling samples of min to during higher than expection condensation point 8 DEG C, often the mobility of sample of fall 2 DEG C observation, read
Until maximum temperature when sample does not flows by 45 DEG C of placement 5s of test tube inclination, this temperature is i.e. condensation point value.
In such scheme step 5, according to oil and gas industry standard SY/T 0520-93, " viscosity of crude measures-rotates
Viscometer counterbalanced procedure ", use viscometer to measure crude oil sample balance apparent viscosity at temperature near condensation point, concrete grammar
It is: at dress sample temperature (i.e. the preparation temperature of emulsion), crude oil sample is loaded in warmed-up measuring cylinder, after constant temperature standing again
Being down to the temperature to be characterized near condensation point with certain rate of temperature fall, constant temperature stands after structure is formed completely, the character of based on crude
With viscometer performance parameter, setting 5 shear rates and measure, each shear rate chooses suitable shear time, until
Each shear rate reaches to shear balance, measures the balance apparent viscosity of crude oil sample.
In such scheme step 6, low-water-content is 1%～10%, and middle moisture content is 30%～40%, high-moisture percentage be 50%～
60%；Low shear rate is 8 r/s～10 r/s, and medium shear rate is 14 r/s～16 r/s, high-rate of shear be 20 r/s～
22 r/s；The low sheraing time is 500s～600s, and middle shear time is 800s～900s, the high shear time be 1100s～
1200s。
The method have the advantages that
1, the present invention sets up the compound method of Simulation of Crude Oil emulsion, prepares the mould identical with the rheological equationm of state under actual production conditions
Intending water-oil emulsion, the rheological behavior for experimentation crude oil emulsion provides basis.
2, the present invention solves the quantization signifying problem of Simulation of Crude Oil emulsion preparation condition.
3, applied thermodynamics of the present invention and the theory of mechanics of viscous fluids, produces description emulsion with VISCOUS FLOW entropy and prepared
The conditional parameter relation of journey, it is achieved that the quantization signifying of each preparation condition parameters relationship of emulsion.
Accompanying drawing explanation
Fig. 1 is Thermogram DSC curve figure in the present invention；
Fig. 2 is the balance apparent viscosity measuring blank crude oil 35 DEG C in the present invention, result figure；
Fig. 3 is the experimental result picture of the emulsion under a kind of preparation condition 35 DEG C in the present invention；
Fig. 4 is to balance the apparent viscosity situation of change figure with moisture content in the present invention；
Fig. 5 is 45 DEG C of experimental result pictures (Newtonian fluid) of the emulsion under a kind of preparation condition in the present invention；
Fig. 6 is 45 DEG C of experimental results (non-Newtonian fluid) of the emulsion under a kind of preparation condition in the present invention.
Detailed description of the invention
The present invention is further illustrated below in conjunction with the accompanying drawings:
This crude oil emulsion compound method based on apparent viscosity quantization signifying is as follows:
Step one: will be after production scene takes crude oil sample to be placed in and transport to laboratory oil drum, according to oil and gas industry
Standard SY/T 0545-2012 " determination of crude oil analysis wax thermal characteristic parameter: differential scanning calorimetry ", uses modulation system differential to sweep
Retouching calorimeter and measure the analysis wax characteristic of crude oil, concrete grammar is: aluminum earthenware inserted by the crude oil sample weighing 4 ~ 8 mg from oil drum
Sealing in crucible, the crucible after sealing puts in the measuring cell of differential calorimetric scan instrument, is heated to 80 DEG C and constant temperature 1min, then with
The rate of temperature fall of 5 DEG C/min is cooled to-20 DEG C from 80 DEG C in a nitrogen atmosphere, in conjunction with Thermogram DSC curve, beginning to deviate from base
The temperature of line is defined as the wax precipitation point WAT of crude oil；With composition between heat flow curve and the baseline of temperature range a certain on curve
Area integral, divided by the average crystallite heat content of wax, obtains the crude oil accumulation analysis wax amount of the following temperature of wax precipitation temperaturec w, available
Following formula calculates:
In formula,The concentration brilliant for separating out wax, wt%；For to measure the temperature of analysis wax amount, DEG C；dQFor temperature fromT +dT
It is down toTTime analysis wax crystallization thermal discharge, J/g；For the average crystallite heat content of wax, depend on the composition of wax, typically take 210J/
g。
Step 2: again measure crude oil sample from oil drum, is heated to oil sample mobility preferably certain temperature, measures
The standard density of dewatered oil, then determine crude oil density at a temperature of its emulsion is prepared by the standard density of crude oil, specific as follows:
(1) according to taken former oil properties, oil sample is heated to the preferable temperature of mobility (such as 50 DEG C)；
(2) the crude oil sample of a certain temperature (such as 50 DEG C) will be risen to, pour in density measure cylinder along inwall carefully, density measure
Cylinder is placed in design temperature (such as 50 DEG C) waters groove, and thermometer is placed in density measure cylinder in oil sample；
(3) densimeter is put in crude oil sample to be measured, after the free floating stable of densimeter, read densimeter and temperature simultaneously
The measurement result of meter；
(4) record the oil sample density of double mensuration, average as this temperature (owing to there being heat to dissipate during measuring
Lose, temperature is as the criterion with temperature reading) under crude oil sample density, and according to following formula calculate crude oil standard density,
Obtain the standard density of crude oilAfter, when can determine crude oil emulsion preparation temperature (such as 45 DEG C) by above-mentioned expression formula
Density
Step 3: taking out crude oil sample again from oil drum and be dispensed into several and seal in port grinding bottles and carry out pretreatment, will should
The sealing port grinding bottle batch filling crude oil sample is put in water-bath simultaneously, stands and is heated to 80 DEG C and constant temperature 2h, takes out above-mentioned sealing
Port grinding bottle stands and naturally cools to room temperature, deposits in variation of ambient temperature smaller part standing more than 48h standby；
Step 4: arbitrarily take out one from step 3 pretreated crude oil sample and seal port grinding bottle, according to petroleum gas
Industry standard SY/T 0541-2009 " condensation point of crude oil algoscopy ", uses petroleum products questionable points instrument to measure condensation point of crude oil, and method is:
After filling sample temperature dress sample more than crude oil wax precipitation point, the rate of temperature fall cooling samples with 0.5～1.0 DEG C/min is solidifying to being higher than expection
Point 8 DEG C time, often fall 2 DEG C observation sample mobility, read until by test tube tilt 45 DEG C place 5s and sample does not flows
Time maximum temperature, this temperature is i.e. condensation point value.
Step 5: further take out several from step 3 pretreated crude oil sample and seal port grinding bottle, according to oil sky
So gas industry standard SY/T 0520-93 " viscosity of crude mensuration-rotating cylinder viscometer counterbalanced procedure ", uses viscometer to measure crude oil and exists
Balance apparent viscosity at temperature near condensation point, concrete grammar is: in dress sample temperature (i.e. preparation temperature T of emulsion, its choosing
Taking is that based on crude analysis wax characteristic determines, temperature TChoose and should be higher than that wax precipitation point, but should not the too high emulsus avoided the formation of
Liquid system is unstable) crude oil sample is loaded in warmed-up measuring cylinder, constant temperature is down to coagulate with certain rate of temperature fall after standing again
Temperature to be characterized near point, constant temperature stands after structure is formed completely, and the character of based on crude and viscometer performance parameter set
5 shear rates measure, and each shear rate chooses suitable shear time, put down until each shear rate reaches to shear
Weighing apparatus, measures the balance apparent viscosity of crude oil sample.
Step 6: be formulated for obtaining the crude oil emulsion that apparent viscosity quantitatively characterizing parameter uses.According to rotary viscosity
The demand of meter laboratory sample selects dosing volume.Concrete grammar is: crude oil sample used is pretreated through step 3, takes
Wherein one bottle put into water-bath airtight be heated to prepare temperature, constant temperature 30 min；By volume moisture contentn w, oil density, water
DensityMeasure the quality of continuous phase and dispersion phase respectively, continuous phase and dispersion phase have been poured into preheated dosing simultaneously and burns
Cup, and use digital display agitator to stir, stirring paddle is placed in beaker central authorities bottom 5mm at the bottom of at the bottom of cup, under a certain stir speed (S.S.)
Stirring sometime, forms the crude oil emulsion needed；
For realizing the purpose of apparent viscosity quantitatively characterizing of the present invention, need to measure different water cut, different stir speed (S.S.) and difference
The crude oil emulsion apparent viscosity of preparation under mixing time, therefore, for making experimental data have typical characteristic, at crude oil emulsion
On the premise of stable system, prepare low (1%～10%), in (30%～40%), the crude oil emulsus of high (50%～60%) 3 moisture content
Liquid, each moisture content crude oil emulsion respectively low (8 r/s～10 r/s), in (14 r/s～16 r/s), high 3(20 r/s
～22 r/s) individual shear rate, low (500s～600s), in (800s～900s), high (1100s～1200s) 3 when shearing
Between, formed under 9 kinds of preparation conditions.
Step 7: determination step six prepares the apparent viscosity of crude oil emulsion, a certain moisture content that step 6 prepares,
Crude oil emulsion under preparation condition carries out crude oil emulsion apparent viscosity mensuration according to the apparent viscosity measuring method of step 5.
After the fresh emulsion prepared loads rheometry cylinder according to measurement standard, residue emulsion is filled to rapidly emulsion steady
In qualitative observation test tube, and it is placed in the program control water-bath of flow graph, makes the emulsion in observation test tube test in flow graph
The sample identical thermal history of experience, to observe in flow graph sample whether breakdown of emulsion.
Measure the apparent viscosity of crude oil emulsion at two temperature: one is preparation temperature, and two is temperature to be characterized；
At a temperature of crude oil emulsion is prepared, owing to, more than wax precipitation point temperature, crude oil normally behaves as Newtonian fluid characteristic, low
Moisture content crude oil emulsion also shows as Newtonian fluid characteristic, need to survey balance apparent viscosity；And the emulsion of middle high-moisture percentage
Showing as non-Newton fluid characteristic, meet power-law fluid constitutive relation, its constitutive equation is as follows, according to apparent viscosity data, intends
Close out crude oil emulsionK 、nValue；
In formulaFor shear stress, Pa；
For shear rate, s-1;
kFor consistency coefficient, Pa sn；
N is rheological behavior index, immeasurable firm amount；
Step 8: according to the condition of step 6 preparation emulsion, calculate the VISCOUS FLOW entropy output value under each preparation condition, suitable
For calculating the expression formula of the low-water-content Newtonian fluid speciality crude emulsion VISCOUS FLOW entropy output value it is
The expression formula of the high-moisture percentage non-Newton fluid characteristic crude oil emulsion VISCOUS FLOW entropy output value be applicable to calculating
In formulaThe volumetric water content of emulsion, %；
、It is respectively water and the density of crude oil, kg/m3；
TThe actual control temperature of agitator tank, i.e. whipping temp, K；
Speed of agitator, r/s；
Metzner constant, takes estimated value 11；
The viscosity of Newtonian fluid, Pa s；
Consistency coefficient in power law model, or power law coefficient, Pa sn；
Liquidity index in power law model, or referred to as power law index, dimensionless；
Mixing time, s；
Emulsion is preparedVISCOUS FLOW entropy in time period produces, J/kg K；
Step 9: the VISCOUS FLOW entropy output value of crude oil emulsion process for preparations g, crude oil analysis wax amount at temperature to be characterizedc w,
Blank crude oil apparent viscosity, the apparent viscosity of crude oil emulsionAnd the shear rate that apparent viscosity measures5 parameters
Meet following relation
In formulaa 0 、a 1 、a 2 、a 3 、a 4Fitting parameter；
By the VISCOUS FLOW entropy output value of each process for preparations g, blank crude oil apparent viscosity, a certain temperature crude oil analysis
Wax amountc w, measure emulsion apparent viscosity time shear rateLogarithm value as the basic data of independent variable, will not
With the emulsion balance apparent viscosity that process for preparation is correspondingLogarithm value as the basic data of dependent variable, to following expression
Formula, utilizes method of least square to carry out linear fit；
Obtain fitting parametera 0 、a 1 、a 2 、a 3 、a 4Value, then above formula is carried out indexation, obtains following expression:
I.e.
(Newtonian fluid)
(non-newtonian flow
Body)
In formulaShear rate, s-1；
Blank viscosity of crude, mpa s；
Crude oil analyses wax amount, % in a certain temperature；
Step 10: under the physical property premises such as known blank oil density, apparent viscosity, analysis wax characteristic, be intended to prepare given moisture content,
The Simulation of Crude Oil emulsion of a certain apparent viscosity at a temperature of determining, according to above-mentioned expression formula, when accurately selecting preparation emulsion
Stirring condition, i.e. according to formulated in combination crude oil based on the apparent viscosity quantization signifying emulsus of different mixing speeds with mixing time
Liquid.
In conjunction with A crude oil, the present invention done further experimental verification as follows:
1., according to step one, measure the analysis wax characteristic of crude oil, gained Thermogram DSC curve such as Fig. 1:
According to the DSC curve shown in Fig. 1, it may be determined that the thermal characteristic parameter of crude oil such as table 1:
Table 1:
| Test oil sample | Wax precipitation temperature/DEG C | Analysis wax peak temperature/DEG C | Paraffin content/m% |
| A crude oil | 37 | 21 | 20.56 |
Accumulation analysis wax scale 2 under portion temperature:
Table 2:
| Temperature/DEG C | Accumulation paraffin content/m% | Temperature/DEG C | Accumulation paraffin content/m% |
| 30 | 1.869 | 35 | 0.340 |
| 31 | 1.539 | 36 | 0.091 |
| 32 | 1.231 | 37 | 0.006 |
| 33 | 0.932 | 38 | 0 |
| 34 | 0.634 |
2., according to step 2, measure the density that crude oil is at 56,54,51 DEG C, and calculate at a temperature of standard density and preparation close
Degree, such as table 3:
Table 3:
| Temperature (DEG C) | Density (kg/m3) |
| 56 | 838.5 |
| 54 | 839.3 |
| 51 | 841 |
| 20 | 843.5 |
| 45 | 845.57 |
3. the dewatered oil pair used by emulsion to be prepared carries out pretreatment.
4., according to step 4, recording condensation point of crude oil is 32.4 DEG C.
5. according to step 5, measuring the balance apparent viscosity of blank crude oil 35 DEG C, result is shown in Fig. 2:
6. according to step 6, preparing emulsion, the concrete preparation condition of emulsion is shown in Table 4:
Table 4:
7. according to step 7, the emulsion under 27 kinds of different preparation conditions can be made altogether, need each emulsion is surveyed
Measuring the apparent viscosity at two temperature: one is preparation temperature (45 DEG C), and two is temperature to be characterized (35 DEG C), location parameter is shown in Table 5:
Table 5:
Fig. 3 be the experimental result of the emulsion 35 DEG C under one of which preparation condition, i.e. speed of agitator be 1000r/min, preparation
Time is 20min, 35 DEG C of apparent viscosity measurement results of the emulsion that moisture content 10% is made into.
Under high, medium and low speed of agitator, stir 20min, the 80s of 35 DEG C of emulsion-1Balance under shear action is apparent
Viscosity is shown in Fig. 4 with the situation of change of moisture content:
Fig. 5 is the 45 DEG C of experimental results of emulsion under one of which preparation condition, i.e. speed of agitator is 1000r/min, during preparation
Between be 20min, 45 DEG C of the emulsion that moisture content 10% is made into, now emulsion is Newtonian fluid.
Thus obtaining the emulsion apparent viscosity under this kind of preparation condition is 50.98mpa s
Fig. 6 is the 45 DEG C of experimental results of emulsion under one of which preparation condition, i.e. speed of agitator is 1000r/min, during preparation
Between be 20min, 45 DEG C of the emulsion that moisture content 50% is made into, now emulsion is non-Newtonian fluid.
According to above apparent viscosity data, simulate formulaIn emulsion under this kind of preparation conditionK
、nValue, is 1.027,0.615 respectively.
8., according to step 8, calculate the VISCOUS FLOW entropy output value under each preparation condition.
9. according to step 9, by the VISCOUS FLOW entropy output value of each process for preparations g, blank crude oil apparent viscosity, certain
The crude oil analysis wax amount of one temperaturec w, measure emulsion apparent viscosity time shear rateLogarithm value as the base of independent variable
Plinth data, by emulsion balance apparent viscosity corresponding for different process for preparationLogarithm value as the basic data of dependent variable,
To formulaMethod of least square is utilized to carry out Linear Quasi
Close, drawa 0、a 1、a 2、a 3、a 4Value, the most respectively 0.84,0.687 ,-0.091,1.049,0.221,
Again above formula is carried out indexation, obtains following expression:
(Newtonian liquid
Body)
(non newtonian
Fluid)
In formulaShear rate, s-1；
Blank viscosity of crude, mpa s；
Crude oil analyses wax amount, % in a certain temperature；
10., under the physical property premises such as known blank oil density, apparent viscosity, analysis wax characteristic, given moisture content, really can be prepared
The Simulation of Crude Oil emulsion of a certain apparent viscosity under fixed temperature, according to above-mentioned expression formula, when can accurately select to prepare emulsion
Stirring condition, i.e. different mixing speeds and the combination of mixing time.
It is 286mpa s(35 DEG C that such as laboratory is intended to by Daqing crude oil preparation apparent viscosity, 80s-1Under shear action)
Two kinds of emulsion of 45.6% moisture content of 17.5% moisture content and 486mpa s, according to the relational expression of step 9, choose low respectively
Rotating speed and high-revolving preparation condition, can extrapolate the preparation time, it is possible to chooses the suitable preparation time, extrapolates preparation and turns
Speed, concrete preparation condition is shown in Table 6:
Table 6:
Claims (6)
1. a crude oil emulsion compound method based on apparent viscosity quantization signifying, it is characterised in that:
Step one: 4 ~ 8 mg will be weighed from oil drum after production scene takes crude oil sample to be placed in and transport to laboratory oil drum
Crude oil sample insert in aluminum cup seal, the crucible after sealing is put in the measuring cell of differential calorimetric scan instrument, is heated to
80 DEG C and constant temperature 1min, then it is cooled to-20 DEG C from 80 DEG C in a nitrogen atmosphere, in conjunction with thermography with the rate of temperature fall of 5 DEG C/min
Figure curve, is defined as the temperature beginning to deviate from baseline the wax precipitation point of crude oil；It is calculated the following temperature of wax precipitation temperature again
Crude oil accumulation analysis wax amountc w；
Step 2: again measure crude oil sample from oil drum, is heated to oil sample mobility preferably certain temperature, measures dehydration
The standard density of crude oil, then the density of crude oil emulsion preparation temperature is determined by the standard density of crude oil；
Step 3: taking out crude oil sample again from oil drum and be dispensed into several and seal in port grinding bottles and carry out pretreatment, will should
The sealing port grinding bottle batch filling crude oil sample is put in water-bath simultaneously, stands and is heated to 80 DEG C and constant temperature 2h, takes out above-mentioned sealing
Port grinding bottle stands and naturally cools to room temperature, deposits in variation of ambient temperature smaller part standing more than 48h standby；
Step 4: arbitrarily take out one from step 3 pretreated crude oil sample and seal port grinding bottle, according to petroleum gas
Industry standard SY/T 0541-2009 " condensation point of crude oil algoscopy ", uses petroleum products questionable points instrument to measure condensation point of crude oil；
Step 5: further take out several from step 3 pretreated crude oil sample and seal port grinding bottle, according to petroleum gas
Industry standard SY/T 0520-93 " viscosity of crude mensuration-rotating cylinder viscometer counterbalanced procedure ", uses viscometer to measure crude oil in condensation point
Balance apparent viscosity at neighbouring temperature；
Step 6: be formulated for obtain apparent viscosity quantitatively characterizing parameter use crude oil emulsion, crude oil sample used be through
Step 3 is pretreated, take wherein one bottle seal port grinding bottle put into water-bath airtight be heated to prepare temperature, constant temperature 30 min；Press
Volumetric water contentn w, oil density, water densityMeasure the quality of continuous phase and dispersion phase respectively, by continuous phase and dispersion
Pouring preheated dosing beaker time identical into, and use digital display agitator to stir, stirring paddle is placed in beaker central authorities bottom away from cup
5mm at the end, stirs sometime under a certain stir speed (S.S.), formed need crude oil emulsion, prepare basic, normal, high 3 aqueous
The crude oil emulsion of rate, each moisture content crude oil emulsion is respectively in basic, normal, high 3 shear rates, basic, normal, high 3 shearings
Time, formed under 9 kinds of preparation conditions；
Step 7: determination step six prepares the apparent viscosity of crude oil emulsion, a certain moisture content that step 6 prepares, preparation
Under the conditions of crude oil emulsion carry out crude oil emulsion apparent viscosity mensuration according to the apparent viscosity measuring method of step 5；Preparation
After good fresh emulsion loads rheometry cylinder according to measurement standard, residue emulsion is filled to rapidly emulsion stability
Observe in test tube, and be placed in the program control water-bath of flow graph, make the emulsion in observation test tube and laboratory sample in flow graph
Experience identical thermal history, to observe in flow graph sample whether breakdown of emulsion；
Measure the apparent viscosity of crude oil emulsion at two temperature: one is preparation temperature, and two is temperature to be characterized；
At a temperature of crude oil emulsion is prepared, owing to, more than wax precipitation point temperature, crude oil normally behaves as Newtonian fluid characteristic, low
Moisture content crude oil emulsion also shows as Newtonian fluid characteristic, need to survey balance apparent viscosity；And the emulsion of middle high-moisture percentage
Showing as non-Newton fluid characteristic, meet power-law fluid constitutive relation, its constitutive equation is as follows, according to apparent viscosity data, intends
Close out crude oil emulsionK 、nValue；
In formulaFor shear stress, Pa；
For shear rate, s-1;
kFor consistency coefficient, Pa sn；
N is rheological behavior index, immeasurable firm amount；
Step 8: according to the condition of step 6 preparation emulsion, calculate the VISCOUS FLOW entropy output value under each preparation condition, suitable
For calculating the expression formula of the low-water-content Newtonian fluid speciality crude emulsion VISCOUS FLOW entropy output value it is:
Be applicable to calculating, the expression formula of the high-moisture percentage non-Newton fluid characteristic crude oil emulsion VISCOUS FLOW entropy output value is:
In this step two formulaThe volumetric water content of emulsion, %；
、It is respectively water and the density of crude oil, kg/m3；
TThe actual control temperature of agitator tank, i.e. whipping temp, K；
Speed of agitator, r/s；
Metzner constant, takes estimated value 11；
The viscosity of Newtonian fluid, Pa s；
Consistency coefficient in power law model, or power law coefficient, Pa sn；
Liquidity index in power law model, or referred to as power law index, dimensionless；
Mixing time, s；
Emulsion is preparedVISCOUS FLOW entropy in time period produces, J/kg K；
Step 9: the VISCOUS FLOW entropy output value of crude oil emulsion process for preparations g, crude oil analysis wax amount at temperature to be characterizedc w, empty
White crude oil apparent viscosity, the apparent viscosity of crude oil emulsionAnd the shear rate that apparent viscosity measures5 parameter symbols
Close following relation
In formulaa 0 、a 1 、a 2 、a 3 、a 4Fitting parameter；
By the VISCOUS FLOW entropy output value of each process for preparations g, blank crude oil apparent viscosity, a certain temperature crude oil analysis wax
Amountc w, measure emulsion apparent viscosity time shear rateLogarithm value as the basic data of independent variable, difference is joined
The emulsion balance apparent viscosity that process processed is correspondingLogarithm value as the basic data of dependent variable, to following formula, profit
Linear fit is carried out with method of least square；
Obtain fitting parametera 0 、a 1 、a 2 、a 3 、a 4Value, then above formula is carried out indexation, obtains following expression:
I.e.
This formula
It is applicable to Newtonian fluid；
This formula is applicable to non-Newtonian fluid；
During this step is variousShear rate, s-1；
Blank viscosity of crude, mpa s；
Crude oil analyses wax amount, % in a certain temperature；
Step 10: under the physical property premises such as known blank oil density, apparent viscosity, analysis wax characteristic, be intended to prepare given moisture content,
The Simulation of Crude Oil emulsion of a certain apparent viscosity at a temperature of determining, according to above-mentioned expression formula, when accurately selecting preparation emulsion
Stirring condition, i.e. according to formulated in combination crude oil based on the apparent viscosity quantization signifying emulsus of different mixing speeds with mixing time
Liquid.
Crude oil emulsion compound method based on apparent viscosity quantization signifying the most according to claim 1, it is characterised in that:
In described step one: according to oil and gas industry standard SY/T 0545-2012, " crude oil analysis wax thermal characteristic parameter is really
Fixed: differential scanning calorimetry ", use modulation system differential scanning calorimeter to measure the analysis wax characteristic of crude oil, concrete grammar is: weigh
The crude oil sample of 4 ~ 8 mg is inserted in aluminum cup and is sealed, and the crucible after sealing is put in the measuring cell of differential calorimetric scan instrument,
Be heated to 80 DEG C and constant temperature 1min, then with the rate of temperature fall of 5 DEG C/min under the nitrogen atmosphere that flow velocity is 50 ml/min from 80
DEG C it is cooled to-20 DEG C, in conjunction with Thermogram DSC curve, the temperature beginning to deviate from baseline is defined as the wax precipitation point WAT of crude oil；With
The area integral of composition between heat flow curve and the baseline of a certain temperature range on curve, divided by the average crystallite heat content of wax,
Analysis wax amount accumulated by crude oil to the following temperature of wax precipitation temperaturec w, calculate by following formula:
In formula,The concentration brilliant for separating out wax, wt%；For to measure the temperature of analysis wax amount, DEG C；dQFor temperature fromT +d T
It is down toTTime analysis wax crystallization thermal discharge, J/g；For the average crystallite heat content of wax, depend on the composition of wax, take 210J/g.
Crude oil emulsion compound method based on apparent viscosity quantization signifying the most according to claim 1 and 2, its feature exists
In: described step 2 determines the density of crude oil emulsion preparation temperatureMethod:
(1) according to taken former oil properties, oil sample is heated to the preferable temperature of mobility, such as 50 DEG C；
(2) will rise to the crude oil sample of a certain temperature, and pour in density measure cylinder along inwall carefully, density measure cylinder is placed in and sets
In the groove of fixed temperature waters, thermometer is placed in density measure cylinder in oil sample；
(3) densimeter is put in crude oil sample to be measured, after the free floating stable of densimeter, read densimeter and temperature simultaneously
The measurement result of meter；
(4) record the oil sample density of double mensuration, average as the crude oil sample density at a temperature of this, and according to
Lower expression formula calculates the standard density of crude oil,
Obtain the standard density of crude oilAfter, density during crude oil emulsion preparation temperature can be determined by above-mentioned expression formula。
4., according to the crude oil emulsion compound method based on apparent viscosity quantization signifying described in claim 1 or 3, its feature exists
In: according to oil and gas industry standard SY/T 0541-2009 " condensation point of crude oil algoscopy " in described step 4, use stone
Oil product condensation point instrument measure condensation point of crude oil, method is: more than crude oil wax precipitation point fill sample temperature dress sample after, with 0.5～1.0 DEG C/
The rate of temperature fall cooling samples of min to higher than expection condensation point 8 DEG C time, often fall 2 DEG C observation sample mobility, read until
Maximum temperature when sample does not flows by 45 DEG C of placement 5s of test tube inclination, this temperature is i.e. condensation point value.
5., according to the crude oil emulsion compound method based on apparent viscosity quantization signifying described in claim 1 or 4, its feature exists
In: in described step 5, according to oil and gas industry standard SY/T 0520-93, " viscosity of crude mensuration-rotating cylinder viscometer is put down
Weighing apparatus method ", use viscometer to measure crude oil sample balance apparent viscosity at temperature near condensation point, concrete grammar is: at dress
Sample temperature, loads crude oil sample in warmed-up measuring cylinder, and constant temperature is down near condensation point with certain rate of temperature fall after standing again
Temperature to be characterized, constant temperature stand after structure is formed completely, the character of based on crude and viscometer performance parameter, set 5 and cut
Cutting speed rate measures, and each shear rate chooses suitable shear time, until each shear rate reaches to shear balance, surveys
Take the balance apparent viscosity of crude oil sample；The preparation temperature of the dress i.e. emulsion of sample temperature.
The most according to claim 1 or 5, crude oil emulsion compound method based on apparent viscosity quantization signifying, its feature exists
In: in described step 6, low-water-content is 1%～10%, and middle moisture content is 30%～40%, and high-moisture percentage is 50%～60%；Low cut
Cutting speed rate is 8 r/s～10 r/s, and medium shear rate is 14 r/s～16 r/s, and high-rate of shear is 20 r/s～22 r/s；
The low sheraing time is 500s～600s, and middle shear time is 800s～900s, and the high shear time is 1100s～1200s.
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