CN102053055B - High-temperature high-pressure multifunctional core sulfur deposition test device and method - Google Patents

Abstract

The invention discloses high-temperature high-pressure multifunctional core sulfur deposition test device and method. The sulfur deposition test device comprises a displacement system, a formation condition analog system, a data acquisition system and a data processing system. The sulfur deposition test method comprises the following steps of: constructing a test environment, measuring the sulfur element deposition on line, observing the sulfur element deposition process on line, and testing the change of permeability of a rock sample before and after sulfur deposition and the like. The invention has the beneficial effects of realizing the visual display of a true core sulfur deposition process, the real-time online measurement of the sulfur deposition and dynamic calculation of core permeability change caused by sulfur deposition and accurately and dynamically evaluating the damage severity of permeability of a reservoir stratum, caused by sulfur deposition in real time, and has the advantages of high degree of automation, good safety, high accuracy, high temperature and high pressure resistance, strong corrosion resistance and the like.

Description

High-temperature high-pressure multifunctional rock core sulphur deposition proving installation and method

Technical field

The present invention relates to a kind of sulphur deposition proving installation and method, particularly relate to a kind of high-temperature high-pressure multifunctional rock core sulphur deposition proving installation and method.

Background technology

High sour gas is ensconced global range and is distributed extensively; For example the gas field, river, ferry of Zhao Lanzhuan gas field, North China, Shengli Oil Field Luo Jia gas field and the Sichuan Basin marine bed of Texas, USA Murray Franklin gas field, Bentz/Bearberry gas field, Canadian Alberta, Panther River gas field, Mississippi, America Black/Josephine gas field, Cox gas field and basin, China Bohai Sea Gulf Continental Facies Stratigraphy flies celestial pass group gas reservoir, gas field, Luo Jia stockaded village and flies celestial pass group gas reservoir, general phosgene Tian Feixian pass group gas reservoir, gas field, iron hillside and fly that celestial pass group gas reservoir, gas field, gantry fly celestial pass group gas reservoir, gas field, field, peak flies celestial pass group gas reservoir, Zhong Ba gas field thunder mouth slope group gas reservoir and Jia Lingjiang River, gas field, river, Wolong group gas reservoir, all belongs to typical high sulfur-bearing reservoir.Because H ₂The existence of S causes high sulfur-bearing gas reservoir recovery features and conventional gas reservoir exploitation characteristic to exist than big-difference.High sulfur-bearing gas reservoir gas is in recovery process, and along with the gas output, reservoir pressure constantly descends; Elementary sulfur will be separated out from carry sulphur gas with monomeric form, and the form with solid-state sulphur exists under suitable temperature conditions, and in the pore constriction of reservoir rock, deposit; Thereby stop up the seepage channel of rock gas, reduce stratum net pore space and permeability, influence the gas production capacity; Like China's North China Oilfield Zhao Lan village gas reservoir, pilot production in 1976, because of insufficient recognition to high sulfur-bearing gas reservoir development; Produce serious elementary sulfur deposition and compelled closing well, operation as yet so far.External J.B.Hyne and G.D.Derdall (1980) have reported the instance of state's elementary sulfur depositions such as Germany, the U.S. and Canada; In case formation temperature is lower than the fusing point of elementary sulfur; Elementary sulfur will deposit, and gas production rate is obviously reduced, and is liquid even elementary sulfur keeps; Because it has bigger viscosity, gas production rate is reduced.B.E.Roberts (1996) and Nacholas Hands (2002) have studied Foothills sulfur-bearing gas field, Rocky Mountains area sulfur deposition characteristic under the shell Canada Company, even sulfur content is lower than 2g/m ³Gas well, do not go out the several months, " sulphur stifled " also can take place, cause production normally to carry out.This shows; The prediction and the assessment technology of sulphur deposition are extremely important to the exploitation of high sulfur-bearing gas reservoir; But generally estimate the sulphur deposition at present according to the changes in solubility of elementary sulfur in rock gas of PVT tube test; True core sulphur is deposited evaluation study almost be in the blank stage, and because sulphur deposition evaluation experimental condition and actual formation seepage flow condition exist than big-difference, the current experiments method of testing can not deposit the extent of injury to reservoir rock sample permeability by accurate in real time dynamic evaluation sulphur.

Summary of the invention

The objective of the invention is to overcome the deficiency of prior art, a kind of high-temperature high-pressure multifunctional rock core sulphur deposition proving installation and method are provided.This device utilizes advanced technique of computer measurement and control and sensor technology; The sulphur deposition forming process of the true rock sample of visual shooting; On-line testing sulphur deposition; Dynamic calculation is because sulphur deposits rerum natura variations such as causing the rock sample permeability etc., and Real-time and Dynamic is estimated the influence that the sulphur deposition causes reservoir damage.

Goal of the invention of the present invention realizes through following technical scheme: high-temperature high-pressure multifunctional rock core sulphur deposition proving installation, it comprises displacement system, formation condition simulation system, data acquisition system (DAS) and data handling system.

The displacement system comprises ST, joins a kind device, gas boosting pump, constant speed and constant pressure pump and intermediate receptacle, and the sample tap of ST is connected with the injection port of joining kind device through pipeline, and the gas boosting delivery side of pump also is connected to the injection port of joining kind device through pipeline; The constant speed and constant pressure delivery side of pump is through the following end entrance of pipeline connection intermediate receptacle, and the gas boosting delivery side of pump also is connected with the last end entrance of intermediate receptacle through pipeline, and the outlet of joining kind device and intermediate receptacle is connected with the formation condition simulation system through pipeline.The constant speed and constant pressure pump is used to provide the continuous no pulse displacement of fluid, ability constant speed, constant voltage work; Intermediate receptacle is a piston type, is used to deposit high-hydrogen sulfide gas appearance, drives the piston of intermediate receptacle through the constant speed and constant pressure pump, with the high-hydrogen sulfide gas appearance displacement that places intermediate receptacle to core holding unit or high pressure form; Join the appearance of joining that kind device is used for test(ing) medium; ST is used to the sample that fetch at the scene that stores, and again sample is changeed appearance and joins appearance to joining in kind device.The gas boosting pump can for the sample supercharging of joining kind device and intermediate receptacle to reach required formation condition.

The formation condition simulation system comprises constant temperature oven, core holding unit and high pressure form.Core holding unit and high pressure form all place in the constant temperature oven, and the injection port of core holding unit and high pressure form is connected with intermediate receptacle with the outlet of joining kind device through intake line.Core holding unit is used for the sulphur deposition mensuration of rock sample and the mensuration of rock sample Permeability Parameters.Core holding unit is processed by titanium alloy, requires its intensity high, in light weight, is used for online weighing; The effect of constant temperature oven is for test formation temperature conditions to be provided; The high pressure form is used for online observation and takes the sulphur deposition process, and the present invention is equipped with a high multiple camera outside the high pressure form, can effectively observe sulphur deposition process in the sand-packed model.

Said high pressure form comprises upper press cover, lower cover, air intake opening, gas outlet, back-up sand cavity, watch window and bracing frame; The back-up sand cavity is fixed on the bracing frame; Air intake opening and gas outlet lay respectively at the two ends of back-up sand cavity and are communicated with; Watch window is positioned at back-up sand cavity top, and upper press cover and lower cover are through being bolted to the top and the bottom of bracing frame.

Data acquisition system (DAS) comprises at least two pressure transducers, temperature sensor, the gentle high-definition camera in on-line metering sky; Pressure transducer places the intake line and the output pipe of core holding unit respectively; The probe of temperature sensor places the middle part of constant temperature oven; Core holding unit is suspended on the suspension hook of on-line metering balance lower end, and high-definition camera places outside the constant temperature enclosure, and the output of pressure transducer, temperature sensor, the gentle high-definition camera in on-line metering sky is connected with data handling system respectively.Pressure transducer and temperature sensor are respectively applied for pressure and the interior temperature of constant temperature oven of measuring the core holding unit two ends, and the on-line metering balance is used for the sulphur deposition that online in real time is measured high-hydrogen sulfide gas stream rock sample when core holding unit; The high definition camera is installed in the constant temperature oven back, through visual window sand-packed model is made a video recording, and is taken by computer control software control.

Data handling system comprises at least one computing machine, places data acquisition board and video frequency collection card and operation data processing software on computers in the computing machine; Computing machine is connected with pressure transducer, temperature sensor and the output of on-line metering balance respectively through the multi pass acquisition mouth of data acquisition board, and computing machine is connected with the output of high-definition camera through video frequency collection card.The data that data processing software on the computing machine is gathered according to the on-line metering balance calculate the sulphur deposition, the candid photograph of Video processing software control high-definition camera action on the computing machine, and the image of capturing preserved and represent.

The displacement system also comprises two wobble pump and a check valve, and hand delivery side of pump is connected with check valve control mouth with the confined pressure mouth of core holding unit respectively through pipeline.The check valve input port is connected with high pressure form output pipe with core holding unit, and the output port of check valve is connected with the separation vessel interface.In two wobble pump, one is used for to the rock sample in the core holding unit confined pressure being provided, and another provides back pressure for check valve, and check valve is used for top hole pressure control, sets up driving pressure differential, makes output pressure steadily to improve measuring accuracy simultaneously.

Data acquisition system (DAS) also comprises the gentle separation vessel in high precision sky, and the high precision balance is connected with separation vessel, and separation vessel is connected with check valve.The high precision balance is used to measure flow quantity.

Data acquisition system (DAS) also comprises at least one flowmeter, and described flow is counted one or more of wide range flowmeter, middle range flowmeter or a small amount of range of flow meter.The inlet end of flowmeter all is connected with the separator gas endpiece through pipeline, and separation vessel is connected with check valve, and the endpiece of flowmeter is connected to neutralization pond through vent line, and the signal system of flowmeter is connected with data acquisition board.

Described constant temperature oven with join kind device outside and be equipped with and isolate the tempered glass cover, the upper end of cloche is provided with hydrogen sulfide gas leakage warning device and explosion-proof exhaust fan.Because hydrogen sulfide gas has severe toxicity; So the present invention has carried out safety prevention measure to whole experimental situation; Promptly an isolation tempered glass cover is installed at constant temperature oven with outside joining kind device; In glass steel cage upper end explosion-proof exhaust fan is installed simultaneously, toxic gas is emptied in the hydrogen sulfide gas absorption tower handle.

Constant temperature oven adopts the heating of totally-enclosed electrothermal tube.Because sulfuretted hydrogen belongs to flammable explosive gas, special strict to environmental requirement, do not allow electric spark; So constant temperature oven of the present invention adopts the hot air convection recycle design; Through the heating of totally-enclosed electrothermal tube required heat is provided, and adopts blower fan to produce recirculating air, form thermal convection.

Each section pipeline of high-temperature high-pressure multifunctional rock core sulphur deposition proving installation of the present invention is equipped with control valve; Be equipped with safety valve in the intake line, described core holding unit is provided with atmospheric valve, and the outlet of atmospheric valve is connected to outside neutralization pond through vent line; Control valve helps control and safeguards; Because poisonous hydrogen sulfide gas can not directly discharge, so the outlet of atmospheric valve is connected to outside neutralization pond through vent line, in neutralization pond, toxic gas is carried out neutralisation treatment; The purpose that safety valve is set is releasing pressure automatically and pump and a pressure transducer realization multiple pressure overload protection when pressure transships, the safety of warranty test personnel and equipment.

The method of high-temperature high-pressure multifunctional rock core sulphur deposition test, it may further comprise the steps:

(1) test environment makes up: set up the test environment of being made up of displacement system, formation condition simulation system, data acquisition system (DAS) and data handling system;

(2) on-line measurement elementary sulfur deposition: at first adopt the on-line metering balance measurement to contain the core holding unit net weight of rock sample before the illogical sour gas appearance.Open valve then; The high-hydrogen sulfide gas appearance that to join in kind device or the intermediate receptacle is injected rock sample; Reduce continuously core holding unit internal temperature or pressure, on-line metering contains the weight of the core holding unit of elementary sulfur deposition rock sample, and the difference of itself and net weight promptly is the sulfur deposition amount;

(3) online observation elementary sulfur deposition process: let the high-hydrogen sulfide gas appearance high pressure form of flowing through, high definition camera see through the visual window shooting high pressure form deposition process of constant temperature oven, and under the control of computing machine candid photograph picture continuously regularly;

(4) the permeability variation test before and after the sulphur deposition: before the illogical sour gas appearance; Earlier with nitrogen test rock sample absolute permeability; The high-hydrogen sulfide gas appearance that to join again in kind device or the intermediate receptacle is injected rock sample; Reduce core holding unit internal temperature or pressure continuously, meanwhile dynamic measurement contains the pressure at elementary sulfur deposition rock sample two ends, calculates viscosity, volume factor and the deviation factors of gas in real time; Calculate the perm-plug method that contains elementary sulfur deposition rock sample in real time according to Darcy's law again, dynamic evaluation sulphur deposition is to the extent of injury of rock sample permeability.

Rock sample perm-plug method computing formula is following:

$K_g=\frac{{2Q}_0{P}_0{\mathrm{\&mu;}}_g{\mathrm{LZ}}_a}{A(P_1^2-{\mathrm{<figure-callout\; id="2"\; label="P"\; filenames="101203204122.png"\; state="\{\{state\}\}">P</figure-callout>}}_2^2)Z_0}---\left(1\right)$

Z _a---the gas Z-factor under test pressure and the probe temperature, decimal;

Z ₀---gas Z-factor under the mark condition condition, decimal;

K _g---perm-plug method, um ²

Q ₀---gas flow under the mark condition condition, cm ³/ s;

L---rock sample length, cm;

A---rock sample cross-sectional area, cm ²

P ₀---atmospheric pressure under the mark condition condition, atm;

P ₁---rock sample intake pressure, atm;

P ₂---rock sample top hole pressure, atm;

μ _g---the gas viscosity under test pressure and the probe temperature, mPa.s.

Z-factor Z in the formula (1) _aCan select strong bearing calibration of Guo Xu and Wichert-Aziz bearing calibration to calculate, its method all is that gas appearance critical parameters are proofreaied and correct, and adopts HTP and DPR Model Calculation mixed gas Z-factor then.

1) the strong bearing calibration of Guo Xu is following to the correction of gas appearance critical parameters:

T _c＝T _m-C _wa (2)

p _c＝T _c∑(x _ip _ci)/[T _c+x ₁(1-x ₁)C _wa] (3)

$T_m=\underset{i=1}{\overset{n}{\mathrm{\&Sigma;}}}\left(x_i{T}_{\mathrm{ci}}\right)---\left(4\right)$

$C_{\mathrm{wa}}=\frac{1}{14.5038}|120\&times;|{(x_1+x_2)}^{0.9}-{(x_1+x_2)}^{1.6}|+15(x_1^{0.5}-x_1^4)|---\left(5\right)$

In the formula: x ₁Be H ₂The mole fraction of S in system;

x ₂Be CO ₂Mole fraction in system.

2) the Wichert-Aziz bearing calibration is following to the correction of gas appearance critical parameters:

T′ _ci＝T _ci-ε (6)

p′ _ci＝p _ciT′ _ci/T _ci (7)

ε＝15(M-M ²)+4.167(N ^0.5-N ²) (8)

In the formula: T _CiBe the critical temperature of i component, K;

P _CiBe the emergent pressure of i component, KPa;

T _Ci' be the correction critical temperature of i component, K;

P _Ci' be the correction emergent pressure of i component, KPa.

M is H in the gaseous mixture ₂S and CO ₂The mole fraction sum;

N is H in the gaseous mixture ₂The mole fraction of S.

The updating formula that mixed gas viscosity calculations model adopts Standing to propose in the formula (1) is:

${\mathrm{\&mu;}}_1^{\&prime;}={\left({\mathrm{\&mu;}}_1\right)}_{\mathrm{un}}+{\mathrm{\&mu;}}_{{\mathrm{<figure-callout\; id="2"\; label="N"\; filenames="101203204122.png"\; state="\{\{state\}\}">N</figure-callout>}}_2}+{\mathrm{\&mu;}}_{{\mathrm{<figure-callout\; id="2"\; label="CO"\; filenames="101203204122.png"\; state="\{\{state\}\}">CO</figure-callout>}}_2}+{\mathrm{\&mu;}}_{H_{2}S}---\left(9\right)$

Each correction coefficient is in the formula:

${\mathrm{\&mu;}}_{H_{2}S}=H_{2}S\&CenterDot;(8.49\&times;{10}^{-3}\lg \left({\mathrm{\&gamma;}}_g\right)+3.73\&times;{10}^{-3})---\left(10\right)$

${\mathrm{\&mu;}}_{{\mathrm{<figure-callout\; id="2"\; label="CO"\; filenames="101203204122.png"\; state="\{\{state\}\}">CO</figure-callout>}}_2}={\mathrm{<figure-callout\; id="2"\; label="CO"\; filenames="101203204122.png"\; state="\{\{state\}\}">CO</figure-callout>}}_2\&CenterDot;(9.08\&times;{10}^{-3}\lg \left({\mathrm{\&gamma;}}_g\right)+6.24\&times;{10}^{-3})---\left(11\right)$

${\mathrm{\&mu;}}_{{\mathrm{<figure-callout\; id="2"\; label="N"\; filenames="101203204122.png"\; state="\{\{state\}\}">N</figure-callout>}}_2}={\mathrm{<figure-callout\; id="2"\; label="N"\; filenames="101203204122.png"\; state="\{\{state\}\}">N</figure-callout>}}_2\&CenterDot;(8.48\&times;{10}^{-3}\lg \left({\mathrm{\&gamma;}}_g\right)+9.59\&times;{10}^{-3})---\left(12\right)$

In the formula:

is sulfuretted hydrogen viscosity correction value, mPas;

is carbon dioxide viscosity correction value, mPas;

is nitrogen viscosity correction value, mPas;

N ₂, CO ₂, H ₂S is respectively the molar content that it accounts for gaseous mixture, decimal;

γ _gBe rock gas relative density (air=1.0);

T is a formation temperature, ℃.

The workflow of high-temperature high-pressure multifunctional rock core sulphur deposition proving installation of the present invention is following:

1) open system's control power supply, system is in and treats duty, presses lighting button, import and top hole pressure button;

2) removal of core clamper from constant temperature oven opens it and packs rock sample to be tested into;

3) core holding unit is put into constant temperature oven, connect pipeline, elder generation presses the rock sample in the core holding unit with wobble pump solid, applies the confined pressure of setting then; Add corresponding back pressure with another wobble pump simultaneously;

4) close the door of constant temperature oven, press blower fan and heat button, set corresponding temperature; After heating a period of time, reach the temperature of setting, need to stablize a period of time, make long core holding unit or high pressure form fully carry out heat interchange, make its temperature reach default value.(note: the machine that necessarily blows in earlier, open heating again, otherwise spot heating caused the damage of system easily! );

5) measurement of rock sample absolute permeability before the sulphur deposition: before the logical sour gas appearance, under certain P and T, earlier with the nitrogen core holding unit of flowing through, according to gas flow and rock sample two ends pressure reduction calculating rock sample absolute permeability;

6) sulphur deposition back rock sample permeability determination: the high-hydrogen sulfide gas appearance that will join in kind device or the intermediate receptacle is injected rock sample; Reduce core holding unit internal temperature or pressure continuously; Elementary sulfur deposition in the on-line metering rock sample, meanwhile dynamic measurement contains the pressure at elementary sulfur deposition rock sample two ends.According to the temperature and pressure of gas composition and system, calculate the viscosity, mu of gas in real time again _g, volume factor B _gWith deviation factors Z _aThen, calculate the corresponding conditions therapeutic method to keep the adverse qi flowing downward in real time according to calculation procedure and survey permeability value, and be kept in the corresponding document automatically.

7) online observation elementary sulfur deposition process: let the high-hydrogen sulfide gas appearance high pressure form of flowing through, high definition camera see through sulphur deposition process in the visual window shooting high pressure form of constant temperature oven, and under computer control candid photograph picture continuously regularly;

8) after experiment test finishes, open antiaircraft valve emptying to neutralization pond and handle high-hydrogen sulfide gas appearance, and with nitrogen rinse-system repeatedly, in case the rock gas corroded pipeline.(note: before closing experimental system, necessarily close earlier and heat Blowing stopper again,, otherwise can cause damage system with abundant heat radiation! );

9) put Laboratory Instruments in order, put instrument and return original position, in order to using next time.

The invention has the beneficial effects as follows: realized true core sulphur deposition forming process visual presentation, sulphur deposition real-time online measuring and cause the dynamic calculation that core permeability changes because of the sulphur deposition; Can estimate the sulphur deposition to the reservoir damage degree by dynamic similation; Have the automaticity height, security is good, accuracy is high, high temperature high voltage resistant, anticorrosive advantage such as strong, temperature and pressure can be respectively up to 150 ℃ with 70MPa.

Description of drawings

Fig. 1 main assembly structural representation of the present invention

Fig. 2 data acquisition of the present invention and control structure synoptic diagram

The structural representation of Fig. 3 high pressure form

Among the figure, 1-ST, 2-are joined a kind device, 3-gas boosting pump, 4-constant speed and constant pressure pump, 5-intermediate receptacle; The 6-constant temperature oven, 7-core holding unit, 8-high pressure form, 9-pressure transducer, 10-on-line metering balance; 11-high precision balance, 12-high-definition camera, 13-wide range flowmeter, 14-data acquisition board, 15-computing machine; The 16-video frequency collection card, 17-wobble pump, 18-check valve, 19-control valve, 20-atmospheric valve; The 21-safety valve, the 22-separation vessel, range flowmeter among the 23-, 24-is the range of flow meter in a small amount, the 25-temperature sensor.The 26-upper press cover, 27-lower cover, 28-air intake opening, 29-gas outlet, 30-back-up sand cavity, 31-watch window, 32-bracing frame.

Embodiment

Further describe technical scheme of the present invention below in conjunction with accompanying drawing: like Fig. 1 high-temperature high-pressure multifunctional rock core sulphur deposition proving installation, it comprises displacement system, formation condition simulation system, data acquisition system (DAS) and data handling system.

Described displacement system comprises ST 1, joins kind device 2, gas boosting pump 3, constant speed and constant pressure pump 4, intermediate receptacle 5, wobble pump 17 and check valve 18; The sample tap of ST 1 is connected with the injection port of joining kind device 2 through pipeline, and the outlet of gas boosting pump 3 also is connected to the injection port of joining kind device 2 through pipeline; The outlet of constant speed and constant pressure pump 4 connects the following end entrance of intermediate receptacle 5 through pipeline; The gas boosting delivery side of pump also is connected with the last end entrance of intermediate receptacle through pipeline; The outlet of joining kind device 2 and intermediate receptacle 5 is connected with the formation condition simulation system through pipeline; The outlet of wobble pump 17 is connected with the confined pressure mouth of core holding unit 7 and the control mouth of check valve 18 respectively through pipeline, and the input port of check valve 18 is connected with the output pipe of core holding unit 7 with high pressure form 8, and the output port of check valve 18 is connected with the interface of separation vessel 22; Join kind device 2 outsides and be provided with isolation tempered glass cover, intermediate receptacle 5 is the piston type container.

Said formation condition simulation system comprises constant temperature oven 6, core holding unit 7 and high pressure form 8; Core holding unit 7 all places in the constant temperature oven 6 with high pressure form 8; The injection port of core holding unit 7 and high pressure form 8 is connected through the last end entrance of intake line with outlet of joining kind device 2 and intermediate receptacle 5; Each of whole device section pipeline is equipped with control valve 19, is equipped with safety valve 21 in the intake line, and described core holding unit 7 is provided with atmospheric valve 20; The outlet of atmospheric valve 20 is connected to outside neutralization pond through vent line; Constant temperature oven 6 adopts the heating of totally-enclosed electrothermal tube, and constant temperature oven 6 outsides are provided with and isolate the tempered glass cover, and the upper end of cloche is provided with hydrogen sulfide gas leakage warning device and explosion-proof exhaust fan.

In order to improve resistance to corrosion, all duct members that contact with hydrogen sulfide gas are the Hastelloy material of anti-sulphur.

Described data acquisition system (DAS) comprises at least two pressure transducers 9, temperature sensor 25, on-line metering balance 10, high precision balance 11, wide range flowmeter 13, middle range flowmeter 23, a small amount of range of flow meter 24, separation vessel 22 and high-definition camera 12; Pressure transducer 9 places the intake line and the output pipe of core holding unit 7 respectively; The probe of temperature sensor 25 places the middle part of constant temperature oven 6; Core holding unit 7 is suspended on the suspension hook of on-line metering balance 10 lower ends; High-definition camera 12 places outside the constant temperature oven 6; The output of pressure transducer 9, temperature sensor 25, on-line metering balance 10 and high-definition camera 12 is connected with data handling system respectively, and high precision balance 11 is connected with separation vessel 22, wide range flowmeter 13, middle range flowmeter 23 and in a small amount range of flow meter 24 inlet end all be connected with separation vessel 22 gas outlet ends through pipeline; Its endpiece is connected to neutralization pond through vent line, and its signal system is connected with data acquisition board (14).

Like Fig. 2; Described data handling system comprises at least one computing machine 15, places data acquisition board 14 and the video frequency collection card 16 in the computing machine 15 and operates in the data processing software on the computing machine 15; Computing machine 15 is connected with pressure transducer 9, temperature sensor 25, outlet metering balance 11, on-line metering balance 10 and wide range flowmeter 13, middle range flowmeter 23 and the output of a small amount of range of flow meter 24 respectively through the multi pass acquisition mouth of data acquisition board 14, and computing machine 15 is connected with the output of high-definition camera 12 through video frequency collection card 16.

Like Fig. 3; High pressure form 8 comprises upper press cover 26, lower cover 27, air intake opening 28, gas outlet 29, back-up sand cavity 30, watch window 31 and bracing frame 32; Back-up sand cavity 30 is fixed on the bracing frame 32; Air intake opening 28 lays respectively at the two ends of back-up sand cavity 30 with gas outlet 29 and is communicated with, and watch window 31 is positioned at back-up sand cavity 30 tops, and upper press cover 26 and lower cover 27 are through being bolted to the top and the bottom of bracing frame 32.

The method of high-temperature high-pressure multifunctional rock core sulphur deposition test, it may further comprise the steps:

(1) test environment makes up: set up the test environment of being made up of displacement system, formation condition simulation system, data acquisition system (DAS) and data handling system;

(2) on-line measurement elementary sulfur deposition: at first adopt on-line metering balance 10 to measure core holding unit 7 net weight that contain rock sample before the illogical sour gas appearance; Open valve then; The high-hydrogen sulfide gas appearance that to join in kind device 2 or the intermediate receptacle 5 is injected rock sample; Reduce continuously core holding unit 7 internal temperatures or pressure, on-line metering contains the weight of the core holding unit of elementary sulfur deposition rock sample, and the difference of itself and net weight promptly is the sulfur deposition amount;

(3) online observation elementary sulfur deposition process: let the high-hydrogen sulfide gas appearance high pressure form 8 of flowing through, high definition camera see through sulphur deposition process in the visual window shooting high pressure form of constant temperature oven 6, and under the control of computing machine 15 candid photograph picture continuously regularly;

(4) the permeability variation test before and after the sulphur deposition: before the illogical sour gas appearance; Earlier with nitrogen test rock sample absolute permeability; The high-hydrogen sulfide gas appearance that to join again in kind device 2 or the intermediate receptacle 5 is injected rock sample; Reduce core holding unit 7 internal temperatures or pressure continuously, meanwhile dynamic measurement contains the pressure at elementary sulfur deposition rock sample two ends, calculates viscosity, volume factor and the deviation factors of gas in real time.Calculate the perm-plug method that contains elementary sulfur deposition rock sample in real time according to Darcy's law again, dynamic evaluation sulphur deposition is to the extent of injury of rock sample permeability.

Claims (1)

1. high-temperature high-pressure multifunctional rock core sulphur deposits proving installation, and it is characterized in that: it comprises displacement system, formation condition simulation system, data acquisition system (DAS) and data handling system;

Described displacement system comprises ST (1), joins a kind device (2), gas boosting pump (3), constant speed and constant pressure pump (4) and intermediate receptacle (5); The sample tap of ST (1) is connected with the injection port of joining a kind device (2) through pipeline, and the outlet of gas boosting pump (3) is parallel to the injection port of joining a kind device (2) through pipeline; The outlet of constant speed and constant pressure pump (4) connects the following end entrance of intermediate receptacle (5) through pipeline; The outlet of gas boosting pump (3) also is connected with the last end entrance of intermediate receptacle (5) through pipeline, and the outlet of joining a kind device (2) and intermediate receptacle (5) is connected with the formation condition simulation system through pipeline;

Said formation condition simulation system comprises constant temperature oven (6), core holding unit (7) and high pressure form (8); Core holding unit (7) and high pressure form (8) all place in the constant temperature oven (6), and the injection port of core holding unit (7) and high pressure form (8) is connected with the outlet of joining a kind device (2) of displacement system and the last end entrance of intermediate receptacle (5) through pipeline;

Said high pressure form (8) comprises upper press cover (26), lower cover (27), air intake opening (28), gas outlet (29), back-up sand cavity (30), watch window (31) and bracing frame (32); Back-up sand cavity (30) is fixed on the bracing frame (32); Air intake opening (28) and gas outlet (29) lay respectively at the two ends of back-up sand cavity (30) and are communicated with; Watch window (31) is positioned at back-up sand cavity (30) top, and upper press cover (26) and lower cover (27) are through being bolted to the top and the bottom of bracing frame (32);

Described data acquisition system (DAS) comprises at least two pressure transducers (9), temperature sensor (25), on-line metering balance (10) and high-definition camera (12); Pressure transducer (9) places the intake line and the output pipe of core holding unit (7) respectively; The probe of temperature sensor (25) places the middle part of constant temperature oven (6); Core holding unit (7) is suspended on the suspension hook of on-line metering balance (10) lower end; High-definition camera (12) places outside the constant temperature oven (6), and pressure transducer (9), temperature sensor (25), on-line metering balance (10) and the output of high-definition camera (12) are connected with data handling system respectively;

Described data handling system comprises at least one computing machine (15), places data acquisition board (14) and the video frequency collection card (16) in the computing machine (15) and operates in the data processing software on the computing machine (15); Computing machine (15) is connected with pressure transducer (9), temperature sensor (25) and the output of on-line metering balance (10) respectively through the multi pass acquisition mouth of data acquisition board (14), and computing machine (15) is connected with the output of high-definition camera (12) through video frequency collection card (16).

2. high-temperature high-pressure multifunctional rock core sulphur deposition proving installation according to claim 1; It is characterized in that: described displacement system also comprises two wobble pump (17) and a check valve (18), and the outlet of wobble pump (17) is connected with the confined pressure mouth of core holding unit (7) and the control mouth of check valve (18) respectively through pipeline; The input port of check valve (18) is connected with the output pipe of core holding unit (7) with high pressure form (8), and the output port of check valve (18) is connected with the interface of separation vessel (22).

3, high-temperature high-pressure multifunctional rock core sulphur deposition proving installation according to claim 2, it is characterized in that: described data acquisition system (DAS) also comprises high precision balance (11), high precision balance (11) is connected with separation vessel (22).

4, high-temperature high-pressure multifunctional rock core sulphur deposition proving installation according to claim 2; It is characterized in that: described data acquisition system (DAS) also comprises at least one flowmeter, and flow is counted one or more of wide range flowmeter (13), middle range flowmeter (23) or a small amount of range of flow meter (24); The inlet end of flowmeter all is connected with separation vessel (22) gas outlet end through pipeline, and the endpiece of flowmeter is connected to neutralization pond through vent line, and the signal system of flowmeter is connected with data acquisition board (14).

5. high-temperature high-pressure multifunctional rock core sulphur deposition proving installation according to claim 1; It is characterized in that: described constant temperature oven (6) and join a kind device (2) outside and be equipped with and isolate the tempered glass cover, the upper end of cloche is provided with hydrogen sulfide gas leakage warning device and explosion-proof exhaust fan.

6. high-temperature high-pressure multifunctional rock core sulphur deposition proving installation according to claim 1, it is characterized in that: described constant temperature oven (6) adopts the heating of totally-enclosed electrothermal tube.

7. high-temperature high-pressure multifunctional rock core sulphur deposition proving installation according to claim 1; It is characterized in that: each of whole device section pipeline is equipped with control valve (19); Be equipped with safety valve (21) in the intake line; Core holding unit (7) is provided with atmospheric valve (20), and the outlet of atmospheric valve (20) is connected to outside neutralization pond through vent line.

8. high-temperature high-pressure multifunctional rock core sulphur deposits method of testing, and it is characterized in that: it may further comprise the steps:

1. test environment makes up: set up based on the test environment of being made up of the described displacement of claim 1 system, formation condition simulation system, data acquisition system (DAS) and data handling system;

2. on-line measurement elementary sulfur deposition: at first adopt on-line metering balance (10) to measure core holding unit (7) net weight that contains rock sample before the logical sour gas appearance; Open valve then; The high-hydrogen sulfide gas appearance that to join in a kind device (2) or the intermediate receptacle (5) is injected rock sample; Reduce continuously core holding unit (7) internal temperature or pressure, on-line metering contains the weight of the core holding unit of elementary sulfur deposition rock sample, and the difference of itself and net weight promptly is the sulfur deposition amount;

3. online observation elementary sulfur deposition process: let the high-hydrogen sulfide gas appearance high pressure form (8) of flowing through; The high definition camera is through sulphur deposition process in the visual window shooting high pressure form of constant temperature oven (6), and picture is captured in timing continuously under the control of computing machine (15);

4. the permeability variation test before and after the sulphur deposition: before the illogical sour gas appearance; Earlier with nitrogen test rock sample absolute permeability; The high-hydrogen sulfide gas appearance that to join again in a kind device (2) or the intermediate receptacle (5) is injected rock sample; Reduce core holding unit (7) internal temperature or pressure continuously, meanwhile dynamic measurement contains the pressure at elementary sulfur deposition rock sample two ends, calculates viscosity, volume factor and the deviation factors of gas in real time; Calculate the perm-plug method that contains elementary sulfur deposition rock sample in real time according to Darcy's law again, dynamic evaluation sulphur deposition is to the extent of injury of rock sample permeability.

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