CN105158212A - Quantitative evaluation system and method of crude oil emulsion stability - Google Patents
Quantitative evaluation system and method of crude oil emulsion stability Download PDFInfo
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Abstract
The invention discloses a quantitative evaluation system and method of a crude oil emulsion stability. The system comprises a signal generator, an oscilloscope, a voltage amplifier, a bottle-test type demulsification dehydrator, a constant-temperature water bath, an emulsion test bottle, a kinetic stability analyzer and a computer, wherein the signal generator generates electric signals with a specific waveform, voltage and frequency, signal amplification is performed through the voltage amplifier, and then an asymmetric high-intensity electric field is applied to crude oil emulsion in the bottle-test type demulsification dehydrator to enable water particles therein to produce electrostatic coalescence and further to accelerate gravity settlement; or under the situation that no electric field is applied, a demulsification agent is directly added into the crude oil emulsion in the bottle-test type demulsification dehydrator to perform chemical demulsification; quantitative analysis and evaluation are performed on the demulsification effect by calculating emulsion dehydration rate or by using the kinetic stability analyzer. The evaluation system and method are convenient, quick, accurate and reliable to use, and can provide convenience for evaluation work of the emulsion demulsification effect under various conditions in laboratories and engineering fields.
Description
Technical field
The present invention relates to a kind of water-in-oil type (w/o type) or oil-in-water type (O/W type) emulsion demulsification technology, particularly relate to a kind of Quantitative Evaluation System and method of crude oil emulsion stability.
Background technology
Inevitably containing a large amount of water and salt in the crude oil exploiting out from stratum, this brings many negative effects to links such as follow-up accumulating, refining processing, therefore general need in oil field to crude oil dewater (salt) process, after refinery then must carry out desalting processing to crude oil, enter atmospheric and vacuum distillation unit again.Water in crude oil mainly contains three kinds of existence forms such as dissolved water, emulsified water, free water, and wherein emulsified water is comparatively stablized and is difficult to adopt conventional standing sedimentation method to remove.People have carried out large quantity research for the breaking emulsion and dewatering problem of crude oil emulsion so far, assist at chemistry on the basis of breakdown of emulsion and propose the measures such as electric field breakdown of emulsion, centrifugal dehydration, microwave, ultrasound wave, UF membrane, but the first-elected electric field breakdown of emulsion of being really used widely in production procedure (or claiming electrostatic coalescence) and the large class of chemical demulsification two, be many times also aided with the measure of heat temperature raising.
At oil-gas gathering and transportation engineering field, along with most of oil field enters the exploitation middle and later periods in the world, secondary, three intensified oil reduction (EOR) technology are applied more prevalent, crude oil in poor quality degree is aggravated, in Produced Liquid, water cut is high, oil-water emulsion fluid viscosity is large, particle water is trickle, the insulating property of emulsion are deteriorated, and causes the Produced Liquid breaking emulsion and dewatering difficulty in oil field ground gathering system constantly to increase.In oil-refining chemical field, along with crude oil heaviness, in poor quality trend serious gradually, add the frequent replacing of refining oil variety, great impact brought to refinery's crude electric desalter, make control crude oil being taken off to rear saliferous index more and more difficult, the variation water quality of Electric Desalting Wastewater is also very large.In order to successfully manage above-mentioned challenge, new and effective emulsion breaker technology and new and effective electric field breaking emulsion and dewatering technology are just becoming the focus of research both at home and abroad, and corresponding emulsion stability and demulsification evaluation method have also been obtained increasing concern.
The method evaluating crude oil emulsion stability has multiple, and main employing at present leaves standstill to observe oil-water separation interface, test critical electric field strength and measure the means such as dehydration rate and studies, and these evaluation methods are subject to Subjective Factors larger in implementation process.The test of different operating personnel or same operation personnel different batches, the test result drawn often has bigger difference, usually needs repeatedly to carry out test of many times, result cause to crude oil emulsion carry out estimation of stability time-consuming, effort, and objectivity is poor, test figure reference value is low.For this reason, many technician to attempt carrying out improvement to the method for estimating stability of crude oil emulsion perfect.
Petroleum drilling rate Insitute, China petroleum drilling Development Institute Zhang Yi proposes a kind of crude cracking and evaluates instrument in patent CN102809562A, and this instrument comprises emulsion preparation facilities, emulsion leaves standstill constant temperature oven and observation device.Be provided with video camera in observation device, emulsion stability process observed, record.Water-oil interface according to observation draw oil and water separation ratio, thus calculate the final dewatering rate of crude oil emulsion, reach the object of Indirect evaluation crude oil emulsion stability.But this device to test process operation is complicated, by visual observation water-oil interface, adopt dehydration rate as characteristic index, result is not accurate enough, and repeatability is lower.China Petroleum Univ. (East-China) Wang Zongxian professor proposes a kind of method evaluating stability of heavy residuum in patent CN102419309A, after heavy oil residue is mixed according to 1:9 ratio with toluene, be heated to 110 DEG C and keep constant temperature 2h, oil sample and bituminous matter wherein are fully dissolved in the middle of toluene, left at room temperature 1h, then in above mixed solution, normal heptane is added according to the ratio of 0.5 ~ 3:10, acutely rock rear rapidly after pour in the cuvette of dried and clean, ultraviolet spectrophotometer is adopted to scan, utilize single sweep operation transmittance, the parameter such as average transmittance and scanning times calculates residual oil stability.Obviously, the method complicated operation, test period reaches more than 3h, and its test with medicament (toluene and normal heptane) is not only expensive, and has certain toxicity, requires higher to the safety guarantee of operating personnel.China Petroleum & Chemical Corporation Research Institute of Petroleum Tan Li proposes a kind of determinator and method of oil-water emulsion stability in patent CN102954983A, and wherein Stability Determination device comprises heating module, electric field controls module and data processing module.By measure in electric field have electric current produce needed for time length and breakdown of emulsion process at the end of the size of current value in electric field, the stability of oil-water emulsion is evaluated.But, because the electrod assembly in electric field controls module is directly exposed in the middle of crude oil emulsion, very easily after water chain is formed, cause short circuit, therefore the evaluation carrying out high-moisture percentage crude oil emulsion stability is not suitable for, and the power of different crude oils emulsion stability qualitatively can only be compared using current value size as measurement mode, cannot show that the direct quantitative of crude oil emulsion stability describes.What favorable to the people teach problem group of China Petroleum Univ. (East-China) proposes a kind of electrostatic coalescence RES(rapid evaluation system) and method in patent CN104515692, and this system is made up of electric supply installation, small-sized electrostatic coalescer and measurement mechanism.The inhomogeneous field being applied some strength by electric supply installation in small-sized electrostatic coalescer implements electric field breakdown of emulsion, digital micrograph is utilized to take pictures and the change of drop particle diameter before and after image processing techniques sample analysis breakdown of emulsion, or utilize the methods analyst subsidence rate of gravity settling, and then evaluate breaking emulsion and dewatering effect.This evaluation system and method obviously have the following disadvantages: one is that digital micrograph is taken pictures the evaluation means that combines with image procossing not only operationally relative complex, and all by the impact of more human factor in microsampling and observation process, the representativeness of drop particle diameter distribution results shows slightly not enough; Two is that digital micrograph shooting technology is poor for the true crude oil emulsion applicability that light transmission is poor; Three is that electrostatic coalescer adopts flat cylindrical structure to design, and be unfavorable for the reading of a small amount of aqueous phase volume in bottom after gravity settling, dehydration rate result of calculation reliability is poor.
Summary of the invention
The object of this invention is to provide a kind of Quantitative Evaluation System convenient to use, crude oil emulsion stability accurately and reliably and method.
The object of the invention is to be achieved through the following technical solutions:
The Quantitative Evaluation System of crude oil emulsion stability of the present invention, comprises signal generator, oscillograph, voltage amplifier, bottle examination type breaking emulsion and dewatering device, constant water bath box, emulsion test bottle, dynamic stability analyser, computing machine etc.;
Electric field breakdown of emulsion or chemical demulsification is carried out by said system:
Described electric field breakdown of emulsion comprises: described signal generator produces the electric signal of specific waveforms, volt value and frequency, carry out after signal amplification through voltage amplifier, non-homogeneous high-strength electric field is applied to the crude oil emulsion in bottle examination type breaking emulsion and dewatering device, make particle water generation electrostatic coalescence wherein, then accelerate gravity settling;
Described chemical demulsification comprises: when not applying electric field, adds emulsion breaker carry out chemical demulsification directly to the crude oil emulsion in described bottle examination type breaking emulsion and dewatering device;
For the emulsion before and after above two kinds of breaking method breakdowns of emulsion, by emulsion dehydration rate, quantitative test and evaluation are carried out to demulsification, or by described dynamic stability analyser and supporting computing machine thereof, quantitative test and evaluation are carried out to demulsification.
Above-mentioned crude oil emulsion stability Quantitative Evaluation System of the present invention realizes the method that crude oil emulsion dynamic stability is evaluated, and comprises step:
A, carry out electric field breakdown of emulsion or chemical demulsification:
A1, electric field breakdown of emulsion: get 50ml crude oil emulsion and be placed in cone end graduated cylinder, produce by signal generator and expect waveform, the electric signal of volt value and frequency, carry out after signal amplification through voltage amplifier, the upper end of coaxal electrode rod in cone end graduated cylinder is inputted by high-tension cable, electrolyte solution is filled in ring cavity outside cone end graduated cylinder, earthing cable immerses in this solution and forms liquid electrode, high-strength electric field heterogeneous is formed between electrode bar and liquid electrode, make the disperse phase particle water generation electrostatic coalescence in crude oil emulsion, apply electric field and be about deenergization after 1min, read the aqueous phase volume bottom cone end graduated cylinder Crude Oil emulsion electric field breakdown of emulsion process moment, contrast with the liquid water content in preliminary crude oil emulsion, corresponding dehydration rate can be calculated,
A2, chemical demulsification: when not applying electric field, chemical demulsification is carried out directly to the emulsion breaker adding variety classes and dosage in cone end graduated cylinder, read the aqueous phase volume bottom cone end graduated cylinder Crude Oil emulsion chemical demulsification process moment, contrast with the liquid water content in preliminary crude oil emulsion, corresponding dehydration rate can be calculated;
B, in electric field breakdown of emulsion or chemical demulsification process moment, take out a certain amount of crude oil emulsion add in the supporting 20mL test bottle of dynamic stability analyser with moving sample pipe, sample liquid height in test bottle is made to be 43mm, then be placed in dynamic stability analyser, after the probe temperature of dynamic stability analyser is adjusted to 35 DEG C automatically, by the function software interface setting program scan pattern of its supporting computing machine;
Described scan pattern comprises: scanning T.T. is 30min, the twice sweep time interval when being 1min, corresponding backscattered light curve and each 30 of the backscattered light change rate curve obtaining crude oil emulsion after the scanning of 30min;
Based on above-mentioned curve, computer calculate draws the steady dynamic mechanics exponential quantity, the settling velocity of disperse phase particle water and the particle size values of disperse phase particle water that reflect test bottle Crude Oil emulsion stability;
C, using stable kinetic index as the critical evaluation parameter evaluating crude oil emulsion stability, with disperse phase particle water settling velocity and disperse phase particle water particle diameter for auxiliary evaluation parameter, steady dynamic mechanics exponential quantity is less, disperse phase particle water settling velocity is slower, disperse phase particle water mean grain size more hour, show that crude oil emulsion stability is higher.
As seen from the above technical solution provided by the invention, the Quantitative Evaluation System of the crude oil emulsion stability that the embodiment of the present invention provides and method, for evaluating crude oil emulsion at different current field condition, dynamic stabilization sex differernce in the situations such as different emulsifiers kind and dosage before and after breakdown of emulsion, realize rapid quantitatively evaluating crude oil demulsification dehydration effect, preferred best breakdown of emulsion parameter, this evaluation system and method are not only convenient to use, and accurately and reliably, can be in laboratory and engineering site the appraisal carrying out various condition emulsified liquid breaking emulsion and dewatering effect and provide convenient.
Accompanying drawing explanation
The structural representation of the Quantitative Evaluation System of the crude oil emulsion stability that Fig. 1 provides for the embodiment of the present invention.
Fig. 2 is the structural representation of bottle examination type breaking emulsion and dewatering device in the embodiment of the present invention.
Fig. 3 is the structural representation of boring end graduated cylinder in the embodiment of the present invention.
In figure, each mark is as follows: 1-signal generator; 2-oscillograph; 3-voltage amplifier; 4-voltage signal line; 5-electric current survey line; 6-bottle examination type breaking emulsion and dewatering device; 7-constant water bath box; 8-emulsion test bottle; 9-dynamic stability analyser; 10-computing machine; 11-high-tension cable; 12-electrode bar; 13-earthing cable; 14-circulating hot water exports; 15-bores end graduated cylinder; 16-circulating hot water; 17-detent; 18-circulating hot water exports; 19-electrolyte solution; 20-crude oil emulsion; 21-positioning end cover.
Embodiment
To be described in further detail the embodiment of the present invention below.
The Quantitative Evaluation System of crude oil emulsion stability of the present invention, its preferably embodiment be:
Comprise signal generator, oscillograph, voltage amplifier, bottle examination type breaking emulsion and dewatering device, constant water bath box, emulsion test bottle, dynamic stability analyser, computing machine etc.;
Electric field breakdown of emulsion or chemical demulsification is carried out by said system:
Described electric field breakdown of emulsion comprises: described signal generator produces the electric signal of specific waveforms, volt value and frequency, carry out after signal amplification through voltage amplifier, non-homogeneous high-strength electric field is applied to the crude oil emulsion in bottle examination type breaking emulsion and dewatering device, make particle water generation electrostatic coalescence wherein, then accelerate gravity settling;
Described chemical demulsification comprises: when not applying electric field, adds emulsion breaker carry out chemical demulsification directly to the crude oil emulsion in described bottle examination type breaking emulsion and dewatering device;
For the emulsion before and after above two kinds of breaking method breakdowns of emulsion, by emulsion dehydration rate, quantitative test and evaluation are carried out to demulsification, or by described dynamic stability analyser and supporting computing machine thereof, quantitative test and evaluation are carried out to demulsification.
When carrying out electric field breakdown of emulsion, the high voltage power supply device that needed for bottle examination type breaking emulsion and dewatering device, high-strength electric field is made up of signal generator and voltage amplifier provides, this electric supply installation can meet the required waveform of test, voltage, frequency, the request for utilization of dutycycle, described voltage amplifier externally provides output end voltage/current monitoring port, voltage detecting end is with the outside output voltage test signal of some minifications of actual output voltage, current output terminal is with the outside output current test signal of certain proportion, by described oscillograph, Real-Time Monitoring is carried out to voltage test signal and current test signal.
Described bottle examination type breaking emulsion and dewatering device comprises high voltage electrode bar, electrolyte solution, earthing cable, outer loop water, cone end graduated cylinder and supporting removable positioning end cover thereof;
Described bottle examination type breaking emulsion and dewatering device defines three liquid and contains region: contain crude oil emulsion in graduated cylinder at the bottom of the cone of internal layer, electrolyte solution is contained in middle open type annular space, recirculated water is contained in outside closed loop space, recirculated water is connected through the gateway of flexible pipe with described constant water bath box with top exit by the bottom inlet on outermost layer housing, form sealing and circulating loop with constant water bath box, guarantee that the temperature of boring crude oil emulsion in end graduated cylinder remains on setting expectation value.
Graduated cylinder lower end at the bottom of described cone is coniform, and indicate volume markings value from top to bottom, the volume of water is deviate from for reading a small amount of crude oil emulsion, described bottle examination type breaking emulsion and dewatering device chassis interior center place is a detent, jointly guarantees that boring end graduated cylinder puts into rear maintenance vertical center attitude with the removable positioning end cover of upper end.
Described bottle examination type breaking emulsion and dewatering device adopts clear glass material processing and fabricating.
Above-mentioned crude oil emulsion stability Quantitative Evaluation System of the present invention realize crude oil emulsion dynamic stability evaluate method, its preferably embodiment comprise step:
A, carry out electric field breakdown of emulsion or chemical demulsification:
A1, electric field breakdown of emulsion: get 50ml crude oil emulsion and be placed in cone end graduated cylinder, produce by signal generator and expect waveform, the electric signal of volt value and frequency, carry out after signal amplification through voltage amplifier, the upper end of coaxal electrode rod in cone end graduated cylinder is inputted by high-tension cable, electrolyte solution is filled in ring cavity outside cone end graduated cylinder, earthing cable immerses in this solution and forms liquid electrode, high-strength electric field heterogeneous is formed between electrode bar and liquid electrode, make the disperse phase particle water generation electrostatic coalescence in crude oil emulsion, apply electric field and be about deenergization after 1min, read the aqueous phase volume bottom cone end graduated cylinder Crude Oil emulsion electric field breakdown of emulsion process moment, contrast with the liquid water content in preliminary crude oil emulsion, corresponding dehydration rate can be calculated,
A2, chemical demulsification: when not applying electric field, chemical demulsification is carried out directly to the emulsion breaker adding variety classes and dosage in cone end graduated cylinder, read the aqueous phase volume bottom cone end graduated cylinder Crude Oil emulsion chemical demulsification process moment, contrast with the liquid water content in preliminary crude oil emulsion, corresponding dehydration rate can be calculated;
B, in electric field breakdown of emulsion or chemical demulsification process moment, take out a certain amount of crude oil emulsion add in the supporting 20mL test bottle of dynamic stability analyser with moving sample pipe, sample liquid height in test bottle is made to be 43mm, then be placed in dynamic stability analyser, after the probe temperature of dynamic stability analyser is adjusted to 35 DEG C automatically, by the function software interface setting program scan pattern of its supporting computing machine;
Described scan pattern comprises: scanning T.T. is 30min, the twice sweep time interval when being 1min, corresponding backscattered light curve and each 30 of the backscattered light change rate curve obtaining crude oil emulsion after the scanning of 30min;
Based on above-mentioned curve, computer calculate draws the steady dynamic mechanics exponential quantity, the settling velocity of disperse phase particle water and the particle size values of disperse phase particle water that reflect test bottle Crude Oil emulsion stability;
C, using stable kinetic index as the critical evaluation parameter evaluating crude oil emulsion stability, with disperse phase particle water settling velocity and disperse phase particle water particle diameter for auxiliary evaluation parameter, steady dynamic mechanics exponential quantity is less, disperse phase particle water settling velocity is slower, disperse phase particle water mean grain size more hour, show that crude oil emulsion stability is higher.
The method is also applicable to the stability analysis of crude oil emulsion before and after centrifugal breakdown of emulsion, microwave demulsifying, the process of ultrasonic dehydration method.
The method is also applicable to comprise the breakdown of emulsion evaluation of water-in-oil type in chemistry, food industry or oil-in-water emulsion;
The method can be screened the kind of emulsion breaker and dosage, also can screen the kind of various emulsifying agent and dosage, can also carry out screening and assessment to the action effect comprising the various emulsion compound methods that mechanical raking is sheared.
Quantitative Evaluation System and the evaluation method of crude oil emulsion stability of the present invention have the following advantages: 1. do not occur with crude oil emulsion in evaluation procedure directly to contact, test operation is convenient, crude oil emulsion consumption is little, single testing cost is low, be both applicable to labs research, is also applicable to engineering site; 2. using dehydration rate or stable kinetic index as evaluation index, test result accurately and reliably, is convenient to realize the transformation from qualitative analysis to quantitative test; 3. be conducive to screening and draw the combination of optimum electric pulse field parameter, most suitable emulsion breaker kind and corresponding optimal dosage.
The present invention can when directly not contacting with emulsion the stability of quick test evaluation crude oil emulsion, and easy and simple to handle, favorable repeatability, ensures that test result has higher accuracy and reliability simultaneously.
The present invention is single mainly for: conventional crude emulsion stability evaluation method characterization method of the prior art, be often confined to qualitative contrast, measure process operation complicated and repeatable low, be unfavorable for evaluating accurately and reliably different breaking method and different breakdown of emulsion setting parameter to deficiencies such as the influence degrees of crude oil emulsion stability, propose a kind of Quantitative Evaluation System and method of crude oil emulsion stability, whether efficient and rational to weigh the method such as electric field breaking emulsion and dewatering or chemical demulsification dehydration, and then promote the progress of the efficient breaking emulsion and dewatering technology of crude oil emulsion.
Based on above guiding theory, the present invention includes high voltage power supply device, bottle examination type breaking emulsion and dewatering device, constant water bath box, emulsion test bottle, dynamic stability analyser, computing machine etc.The vertical structure layout of bottle examination type breaking emulsion and dewatering device substantially in three cylinder coaxial inner conductors, splendid attire crude oil emulsion to be tested in graduated cylinder at the bottom of the cone of innermost layer, annular space splendid attire electrolyte solution between cone end graduated cylinder and middle cylinder, the annular space splendid attire recirculated water between middle cylinder and cylindric outer cylinder body.Gateway on cylindric outer cylinder body is connected with constant water bath box by two sections of flexible pipes, forms closed circuit to keep the temperature of crude oil emulsion to be tested in middle level annular space internal electrolyte solution and cone end graduated cylinder substantially constant near setting value.High voltage electrode bar and ground-electrode are inserted respectively in the crude oil emulsion in cone end graduated cylinder and the electrolyte solution in the annular space of middle level, open the high voltage power supply device be connected with high voltage electrode bar, just can apply non-homogeneous high-strength electric field to the crude oil emulsion in cone end graduated cylinder, make it that electric field breaking emulsion and dewatering occur.Also can when not applying electric field, the emulsion breaker adding variety classes and dosage in cone end graduated cylinder carries out chemical demulsification.Crude oil emulsion after implementing breakdown of emulsion is left standstill a period of time, the water deviate from just can be deposited in bottom cone end graduated cylinder, because cone end graduated cylinder adopts clear glass material and indicates with volume scale, therefore directly can read the volume of electric field breakdown of emulsion or chemical demulsification early, middle, late stage bottom aqueous phase, and then by the dehydration rate calculated, quantitative test and evaluation be carried out to demulsification.
What is more important, the present invention proposes to sample the crude oil emulsion of boring certain height place in end graduated cylinder before and after electric demulsification or chemical demulsification respectively, utilizes analysis of stability analyzer to carry out the quantitative analysis evaluation of emulsion stability.Described analysis of stability analyzer preferential recommendation adopts Turbiscan series dynamic laser granularity and the analysis of stability analyzer of French Formulaction company, based on " program scanning pattern; using the backward scattering light value of first time scanning gained crude oil emulsion as reference standard, in succession obtain backscattered light rate of change Δ BS (%) remaining crude oil emulsion in sweep time.Through supporting function software to after the process of Δ BS infinitesimal analysis, can be exchanged into dynamic stabilization index (TSI) value setting crude oil emulsion in sweep time, thus be that the stability evaluating emulsion provides powerful support.
The evaluation test of inventor's industry ongoing substantial oil emulsion stability indoor test proves, tool of the present invention has the following advantages:
1, do not occur directly to contact with crude oil emulsion in evaluation procedure, test operation is convenient, crude oil emulsion consumption is little, single testing cost is low, is applicable to the test evaluation service of laboratory or engineering site;
2, using dehydration rate or dynamic stabilization index as evaluation index, test result accurately and reliably, is convenient to realize the transformation from qualitative analysis to quantitative test;
3, bottle examination type electrostatic coalescer adopts clear glass material, innermost layer is the graduated cylinder of cone bottom structure and indicates with volume scale, be convenient to the deposition dehydrating situation of emulsion in real-time monitored breakdown of emulsion process, the forward and backward bottom aqueous phase bulking value of accurate reading breakdown of emulsion, to calculate dehydration rate, is conducive to screening and draws the combination of optimum electric pulse field parameter, most suitable emulsion breaker kind and corresponding optimal dosage;
4, be not only applicable to crude oil emulsion, be also applicable to the breakdown of emulsion evaluation comprising the industrial all kinds of water-in-oil type (w/o type) such as chemistry, food or oil-in-water type (O/W type) emulsion; Both can screen the kind of emulsion breaker and dosage, also can screen the kind of various emulsifying agent and dosage, even can carry out screening and assessment to the action effect comprising the various emulsion compound methods that mechanical raking is sheared.
Specific embodiment:
As shown in Figure 1, Figure 2, Figure 3 shows, the Quantitative Evaluation System of crude oil emulsion stability is made up of signal generator (1), oscillograph (2), voltage amplifier (3), bottle examination type breaking emulsion and dewatering device (6), constant water bath box (7), emulsion test bottle (8), dynamic stability analyser (9), computing machine (10) etc., and signal generator (1), oscillograph (2), voltage amplifier (3) form high-tension electricity supply and supervising device jointly.The vertical structure layout of bottle examination type breaking emulsion and dewatering device (6) substantially in three cylinder coaxial inner conductors, splendid attire crude oil emulsion to be tested (20) in graduated cylinder (15) at the bottom of the cone of innermost layer, middle level annular space splendid attire electrolyte solution (19) between cone end graduated cylinder (15) and middle cylinder, the outer annular space splendid attire recirculated water between middle cylinder and cylindric outer cylinder body.Gateway on cylindric outer cylinder body is connected with constant water bath box by two sections of flexible pipes, forms closed circuit to keep the temperature of crude oil emulsion to be tested (19) in middle level annular space internal electrolyte solution (20) and cone end graduated cylinder substantially constant near setting value.Bottle examination type breaking emulsion and dewatering device (6) chassis interior center place is a small-sized detent (17), be aided with the removable positioning end cover in upper end (21), jointly guarantee that cone end graduated cylinder (15) puts into rear maintenance vertical center attitude.Cone end graduated cylinder (15) adopts Upper cylindrical-lower cone combination, and indicates volume markings value from top to bottom, is convenient to read the volume that a small amount of crude oil emulsion deviates from water.Voltage amplifier (3) externally provides output end voltage/current monitoring port, voltage detecting end is with some minifications (as 1/1000) of actual output voltage outwards output voltage test signal, current output terminal, with certain proportion (as 1V/12mA) outwards output current test signal, uses oscillograph to carry out Real-Time Monitoring to voltage test signal and current test signal.
In practical operation, signal generator (1) produces specific waveforms, the electric signal of frequency and voltage, inputted the upper end of coaxal electrode rod (12) in cone end graduated cylinder (15) in bottle examination type breaking emulsion and dewatering device (6) by high-tension cable (11) after voltage amplifier (3) amplifies, earthing cable (13) immerses in electrolyte solution (19) and forms liquid electrode, so just, between coaxal electrode rod (12) and liquid electrode, form non-homogeneous high-strength electric field, make the particle water generation electrostatic coalescence in crude oil emulsion (20), then there is gravity settling.Also when not applying electric field, chemical demulsification can be carried out directly to the emulsion breaker adding variety classes and dosage in the crude oil emulsion (20) in cone end graduated cylinder (15).Then according to the concrete condition of different use occasion and crude oil emulsion, to two kinds of evaluation methods, (one is utilize analysis of stability analyzer to obtain the forward and backward stable kinetic index of breakdown of emulsion, two is directly read the forward and backward bottom aqueous phase volume of breakdown of emulsion, obtain emulsion dehydration rate) carry out reasonable selection, and then quantitative test and evaluation are carried out to the emulsion stability after breakdown of emulsion process or demulsification, for the screening of optimum breakdown of emulsion parameter provides reference frame accurately.
Embodiment one: evaluate the impact of different electric pulse field parameter on crude oil emulsion stability.
1, the same batch of crude oil emulsion (about 50ml) prepared is poured in graduated cylinder (15) at the bottom of the cone of bottle examination electrostatic coalescer (6), under circulator bath effect, rise to setting breakdown of emulsion temperature; Then high-tension electricity supply and supervising device is opened, in the crude oil emulsion (20) in cone end graduated cylinder (15), apply the inhomogeneous field of high strength, make the disperse phase particle water generation electrostatic coalescence in crude oil emulsion (20).After the time of continued power about 1min, close high-tension electricity supply and supervising device.Crude oil emulsion after implementing breakdown of emulsion is left standstill a period of time, the water deviate from just can be deposited in the bottom of cone end graduated cylinder (15), because cone end graduated cylinder (15) adopts clear glass material and indicates with volume scale, therefore directly and comparatively adequately can read the volume of bottom aqueous phase before and after electric field breakdown of emulsion, and then by the dehydration rate calculated, quantitative test and evaluation be carried out to demulsification.
2, use prepare the crude oil emulsion before electric field breakdown of emulsion, or use transfer pipet to take out the crude oil emulsion (about 17ml) after electric field breakdown of emulsion apart from liquid level certain depth in cone end graduated cylinder (15), added in the supporting 20mL test bottle (8) of French Formulaction company's T urbiscan analysis of stability analyzer (9), make sample liquid height in test bottle (8) be about 43mm (actual volume is about 17mL), be placed in Turbiscan analysis of stability analyzer (9).The measuring sonde of Turbiscan analysis of stability analyzer (9) is made up of a pulsed near infrared light source (wavelength 880nm) and two synchronous fluorescence detectors, and two optical detectors detect the intensity of collecting the transmitted light through sample and the backscattered light by sample reflection (departing from incident light 135 ° place) respectively.Due to transmitted light that detecting device obtains and backscattered light intensity (luminous flux, represent with %) directly by concentration (percent by volume) and the mean diameter decision of sample dispersion phase, therefore by continuing a certain cross section of scanning samples, to obtain on this cross section backscattered light flux BS and transmitted light flux T-phase to the change curve of time, just can know the change of sample at this section concentration or grain diameter.The Data Collection mode of Turbiscan analysis of stability analyzer (9) is divided into two kinds, one is " program scanning pattern ": every 40 μm of the scanning height along 55mm collects a secondary data, every 20s does 1 time and scans and collect data at ambient temperature, and within every 30 seconds, temperature controls once; Two is " fixed position pattern ", and on a selected height of specimen, p.s. measures once.
Starting up Turbiscan analysis of stability analyzer (9), after instrument probe temperature to be analyzed is adjusted to design temperature (35 DEG C) voluntarily, in its supporting computing machine (10) software interface, " program scanning pattern " is set, light scanning T.T. is 30min, and the twice sweep time interval is 1min.Due to the transmitted intensity T<0.2% of crude oil emulsion, the luminous flux BS (%) often choosing backscattered light is measurement index.Using the backward scattering light value that draws of first time test crude oil emulsion as reference standard, the backward scattering light value BS (%) in residue sweep time and the difference (i.e. backscattered light rate of change Δ BS (%)) between reference standard are as intuitively reflecting the stability change situation of sample in observation time.Accumulative backscattered light curve and each 30 of the backscattered light change rate curve obtaining crude oil emulsion, based on above-mentioned curve, through TurbiscanEasysoft software, infinitesimal analysis process is done to Δ BS (%), be converted into the numerical value of average backscattered light rate of change in specific trace interval, with Turbiscan dynamic stabilization index (TurbiscanStabilityIndex, TSI) represent, the particle size values of disperse phase drops of water fall down speed and disperse phase water droplet in crude oil emulsion can also be obtained simultaneously.And then quantitative test and evaluation are carried out to the stability of emulsion or electric field demulsification.
3, change the setting value (comprising voltage, frequency, peak pulse duration etc.) of signal generator (1) signal parameter and electric field action time etc., carry out the mensuration of dynamic stability parameter or dehydration rate after crude oil emulsion breaking emulsion and dewatering under different electric pulse field parameter according to step described in 1-2.By orthogonal test and single factor experiment, rapid screening goes out to have the electric pulse field parameter of best demulsification.
Embodiment two: evaluation emulsion breaker kind and dosage are on the impact of crude oil emulsion dynamic stability.
Be with embodiment one difference, electric field is not applied to bottle examination type breaking emulsion and dewatering device in the present embodiment, and adopt emulsion breaker directly to carry out chemical demulsification to crude oil emulsion in cone end graduated cylinder (15), and then crude oil emulsion dynamic stability or demulsification after assay chemical demulsification.Embodiment is as follows:
1, the same batch of crude oil emulsion (about 50ml) prepared is poured in graduated cylinder (15) at the bottom of the cone of bottle examination type breaking emulsion and dewatering device (6), rise to setting breakdown of emulsion temperature under circulator bath effect after, the emulsion breaker adding particular types and dosage in cone end graduated cylinder (15) carries out chemical demulsification, and the measure such as can be aided with stirring if desired, rock is to promote emulsion breaker and crude oil emulsion contact reaction more equably.
2, use prepare the crude oil emulsion before chemical demulsification, or use transfer pipet to take out the crude oil emulsion (about 17ml) after chemical demulsification apart from liquid level certain depth in cone end graduated cylinder (15), with reference to the method in embodiment one described in step 2, by Turbiscan analysis of stability analyzer (9), determination and analysis is carried out to crude oil emulsion, obtain the crude oil emulsion dynamic stability data before and after chemical demulsification.
3, by changing emulsion breaker kind and addition, the assay of dynamic stability parameter and demulsification before and after crude oil emulsion breakdown of emulsion under different emulsion breaker kind and dose profile is carried out according to step described in 1-2.By orthogonal test and single factor experiment, rapid screening goes out to have emulsion breaker type and the additive capacity thereof of best demulsification.
The above; be only the present invention's preferably embodiment, but protection scope of the present invention is not limited thereto, is anyly familiar with those skilled in the art in the technical scope that the present invention discloses; the change that can expect easily or replacement, all should be encompassed within protection scope of the present invention.Therefore, protection scope of the present invention should be as the criterion with the protection domain of claims.
Claims (8)
1. the Quantitative Evaluation System of a crude oil emulsion stability, it is characterized in that, comprise signal generator (1), oscillograph (2), voltage amplifier (3), bottle examination type breaking emulsion and dewatering device (6), constant water bath box (7), emulsion test bottle (8), dynamic stability analyser (9), computing machine (10);
Electric field breakdown of emulsion or chemical demulsification is carried out by said system:
Described electric field breakdown of emulsion comprises: described signal generator (1) produces the electric signal of specific waveforms, volt value and frequency, after voltage amplifier (3) carries out signal amplification, non-homogeneous high-strength electric field is applied to the crude oil emulsion in bottle examination type breaking emulsion and dewatering device (6), make particle water generation electrostatic coalescence wherein, then accelerate gravity settling;
Described chemical demulsification comprises: when not applying electric field, adds emulsion breaker carry out chemical demulsification directly to the crude oil emulsion in described bottle examination type breaking emulsion and dewatering device (6);
For the emulsion before and after above two kinds of breaking method breakdowns of emulsion, by emulsion dehydration rate, quantitative test and evaluation are carried out to demulsification, or by the function software of described dynamic stability analyser (9) and sub computers (10) thereof, quantitative test and evaluation are carried out to demulsification.
2. crude oil emulsion stability Quantitative Evaluation System according to claim 1, it is characterized in that, when carrying out electric field breakdown of emulsion, the high voltage power supply device that the required high-strength electric field of bottle examination type breaking emulsion and dewatering device (6) is made up of signal generator (1) and voltage amplifier (3) provides, this electric supply installation can meet the required waveform of test, voltage, frequency, the request for utilization of dutycycle, described voltage amplifier (3) externally provides output end voltage/current monitoring port, voltage detecting end is with the outside output voltage test signal of some minifications of actual output voltage, current output terminal is with the outside output current test signal of certain proportion, by described oscillograph (2), Real-Time Monitoring is carried out to voltage test signal and current test signal.
3. crude oil emulsion stability Quantitative Evaluation System according to claim 1, it is characterized in that, described bottle examination type breaking emulsion and dewatering device (6) comprises high voltage electrode bar (12), electrolyte solution (19), earthing cable (13), outer loop water (16), cone end graduated cylinder (15) and supporting removable positioning end cover (21) thereof, described bottle examination type breaking emulsion and dewatering device (6) defines three liquid and contains region: contain crude oil emulsion (20) in graduated cylinder (15) at the bottom of the cone of internal layer, electrolyte solution (19) is contained in middle open type annular space, recirculated water (16) is contained in outside closed loop space, recirculated water is connected through the gateway of flexible pipe with described constant water bath box (7) with top exit (14) by the bottom inlet (18) on outermost layer housing, sealing and circulating loop is formed with constant water bath box (7), guarantee that the temperature of boring end graduated cylinder (15) interior crude oil emulsion (20) remains on setting expectation value.
4. crude oil emulsion stability Quantitative Evaluation System according to claim 3, it is characterized in that, at the bottom of described cone, graduated cylinder (15) lower end is coniform, and indicate volume markings value from top to bottom, the volume of water is deviate from for reading a small amount of crude oil emulsion, described bottle examination type breaking emulsion and dewatering device (6) chassis interior center place is a detent (17), jointly guarantees that boring end graduated cylinder (15) puts into rear maintenance vertical center attitude with the removable positioning end cover (21) of upper end.
5. the crude oil emulsion stability Quantitative Evaluation System according to any one of claim 1-4, is characterized in that, described bottle examination type breaking emulsion and dewatering device (6) adopts clear glass material processing and fabricating.
6. the crude oil emulsion stability Quantitative Evaluation System described in any one of claim 1-5 realizes the method that crude oil emulsion dynamic stability is evaluated, and it is characterized in that, comprises step:
A, carry out electric field breakdown of emulsion or chemical demulsification:
A1, electric field breakdown of emulsion: get 50ml crude oil emulsion and be placed in cone end graduated cylinder (15), produce by signal generator (1) and expect waveform, the electric signal of volt value and frequency, after voltage amplifier (3) carries out signal amplification, the upper end of cone end graduated cylinder (15) interior coaxal electrode rod (12) is inputted by high-tension cable (11), electrolyte solution (19) is filled in cone end graduated cylinder (15) ring cavity outward, earthing cable (13) immerses in this solution and forms liquid electrode, high-strength electric field heterogeneous is formed between electrode bar (12) and liquid electrode, make the disperse phase particle water generation electrostatic coalescence in crude oil emulsion (20), apply electric field and be about deenergization after 1min, read the aqueous phase volume bottom cone end graduated cylinder (15) Crude Oil emulsion electric field breakdown of emulsion process moment, contrast with the liquid water content in preliminary crude oil emulsion, corresponding dehydration rate can be calculated,
A2, chemical demulsification: when not applying electric field, chemical demulsification is carried out directly to the emulsion breaker adding variety classes and dosage in cone end graduated cylinder (15), read the aqueous phase volume bottom cone end graduated cylinder (15) Crude Oil emulsion chemical demulsification process moment, contrast with the liquid water content in preliminary crude oil emulsion, corresponding dehydration rate can be calculated;
B, in electric field breakdown of emulsion or chemical demulsification process moment, take out a certain amount of crude oil emulsion (20) add in the supporting 20mL test bottle (8) of dynamic stability analyser (9) with moving sample pipe, sample liquid height in test bottle (8) is made to be 43mm, then be placed in dynamic stability analyser (9), after the probe temperature of dynamic stability analyser (9) is adjusted to 35 DEG C automatically, by the function software interface setting program scan pattern of its supporting computing machine (10);
Described scan pattern comprises: scanning T.T. is 30min, the twice sweep time interval when being 1min, corresponding backscattered light curve and each 30 of the backscattered light change rate curve obtaining crude oil emulsion after the scanning of 30min;
Based on above-mentioned curve, computing machine (10) calculates the steady dynamic mechanics exponential quantity, the settling velocity of disperse phase particle water and the particle size values of disperse phase particle water that reflect test bottle Crude Oil emulsion stability;
C, using stable kinetic index as the critical evaluation parameter evaluating crude oil emulsion stability, with disperse phase particle water settling velocity and disperse phase particle water particle diameter for auxiliary evaluation parameter, steady dynamic mechanics exponential quantity is less, disperse phase particle water settling velocity is slower, disperse phase particle water mean grain size more hour, show that crude oil emulsion stability is higher.
7. crude oil emulsion stability method for quantitatively evaluating according to claim 6, is characterized in that, the method is also applicable to the stability analysis of crude oil emulsion before and after centrifugal breakdown of emulsion, microwave demulsifying, the process of ultrasonic dehydration method.
8. crude oil emulsion stability method for quantitatively evaluating according to claim 6, is characterized in that, the method is also applicable to comprise the breakdown of emulsion evaluation of water-in-oil type in chemistry, food industry or oil-in-water emulsion;
The method can be screened the kind of emulsion breaker and dosage, also can screen the kind of various emulsifying agent and dosage, can also carry out screening and assessment to the action effect comprising the various emulsion compound methods that mechanical raking is sheared.
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