CN104568678A - Device and method for testing gas-liquid sulfur phase permeation curve of high-temperature high-pressure high-sulfur-content gas reservoir - Google Patents

Abstract

The invention discloses a device and a method for testing a gas-liquid sulfur phase permeation curve of a high-temperature high-pressure high-sulfur-content gas reservoir. The testing device comprises a displacement system, a stratum condition simulation system, a back-pressure system, a data testing system and a data acquisition system. The testing method comprises the following steps: selecting and treating a rock core; preparing rock core saturated stratum water and liquid sulfur; simulating a high-temperature and high-pressure environment of the stratum; determining the condition of liquid sulfur phase permeability under irreducible water saturation; performing a phase permeation test on filling of gas-liquid sulfur according to a set ratio; recording the amount VSi of liquid sulfur and the gas amount Vgi generated totally; correcting the stratum condition; calculating the relative permeability Krs of the liquid sulfur phase, the relative permeability Krg of the gas phase and the gas saturation Sg of a rock sample at each moment and the like. The device and the method disclosed by the invention can be used for safely, conveniently, rapidly, accurately and efficiently measuring the high-temperature high-pressure gas-liquid sulfur phase permeation data and providing scientific data support for making a reasonable development scheme for the high-sulfur-content gas reservoir.

Description

High Temperature High Pressure acid gas reservoir gas-liquid sulphur phase percolation curve proving installation and method

Technical field

The present invention relates to petroleum natural gas exploration technical field, particularly relate to a kind of the High Temperature High Pressure solution-air sulphur phase percolation curve proving installation and the method that meet acid gas reservoir Development and Production reality.

Background technology

Acid gas reservoir distribution on global is extensive, the whole world has found more than 400 the high sulfur Gas Fields with commercial value at present, and it is mainly distributed in Canada, the U.S., France, Germany, Russia, China and Middle East.Whole world acid gas reservoir reserves are more than 736320 × 108m ³, account for 40% of world's rock gas total reserves.China's Sichuan Basin Northeast Sichuan area aboundresources, such as, flies the Dukouhe of celestial pass group and Changxing Group, iron hillside, general light, Long Gang, Yuan Ba, Luo Jiazhai, the Temple of the Dragon King etc. and is acid gas reservoir.Acid gas reservoir gas is in recovery process, along with gas output, reservoir pressure constantly declines, and elementary sulfur will be separated out from carrying sulphur gas with monomeric form, when temperature exists with the form of molten sulfur higher than 120 DEG C, now in porous medium, fluid flowing is solution-air sulphur Multiphase Flow.

But, in current field of oil development, liquid phase oozes method of testing Main Basis standard SY/T5345-2007 " in rock two-phase fluid relative permeability assay method ", steady state method or cold store enclosure is adopted to record, experimental study is oozed mutually to true core solution-air sulphur and is in the blank stage, and existing air water oozes laboratory experiment condition mutually and true stratum filtration condition exists larger difference, and solution-air sulphur can not be met ooze condition mutually, the precision deficiency etc. of existing measuring equipment, causes existing experimental provision cannot measure solution-air sulphur phase percolation curve at all simultaneously.Therefore be necessary to improve existing equipment and provide a kind of solution-air sulphur meeting acid gas reservoir production actual to ooze proving installation and method mutually.

Summary of the invention

The object of the invention is to overcome the deficiencies in the prior art, High Temperature High Pressure acid gas reservoir gas-liquid sulphur phase percolation curve proving installation and method are provided, High Temperature High Pressure solution-air sulphur can be measured safe, convenient, fast, accurately and efficiently and ooze data mutually, for acid gas reservoir formulates the Data support that rational development plan provides science.

The object of the invention is to be achieved through the following technical solutions: High Temperature High Pressure acid gas reservoir gas-liquid sulphur phase percolation curve proving installation, it comprises displacement system, formation condition simulation system, back pressure system, data acquisition system (DAS) and data testing system.

Described displacement system comprises sulfur-containing gas sample pot, nitrogen pot, gas boosting pump, gas sample intermediate receptacle, the first constant speed and constant pressure pump, molten sulfur intermediate receptacle, water sample intermediate receptacle, the second constant speed and constant pressure pump and filtrator.

Described formation condition simulation system comprises core holding unit, automatically confined pressure and follows the trail of pump and constant temperature oven.

Described back pressure system comprises back pressure control valve and backpressure pump.

Described data testing system comprises high precision magnetic levitation balance, high temperature high voltage resistant gas-liquid separator, conical flask, condensation bath, gas meter and tail gas neutralization pond.

Described data acquisition system (DAS) comprises multiple pressure transducer, temperature sensor, Thermostat Temperature Control instrument, gas meter, magnetic suspension balance sensor, data acquisition board and computing machine.

First constant speed and constant pressure delivery side of pump end is connected with the inlet end of gas sample intermediate receptacle, the endpiece of gas sample intermediate receptacle is connected with the inlet end of gas boosting delivery side of pump end and core holding unit respectively, and gas boosting delivery side of pump end is connected with the endpiece of sulfur-containing gas sample pot and nitrogen pot respectively.

Second constant speed and constant pressure delivery side of pump end is connected with the inlet end of water sample intermediate receptacle and molten sulfur intermediate receptacle respectively, the endpiece of water sample intermediate receptacle is connected with the inlet end of core holding unit, and the endpiece of molten sulfur intermediate receptacle is connected with the inlet end of core holding unit by filtrator.

The endpiece of core holding unit is connected with the inlet end of high temperature high voltage resistant gas-liquid separator and back pressure control valve respectively, the endpiece of back pressure control valve is connected with the inlet end of backpressure pump, automatic confined pressure is followed the trail of delivery side of pump end and is connected with the confined pressure input end of core holding unit, the liquid outlet end of high temperature high voltage resistant gas-liquid separator is connected with the inlet end of conical flask, conical flask hangs on high precision magnetic levitation balance, the inlet end that gas outlet end and the condensation of high temperature high voltage resistant gas-liquid separator are bathed is connected, the endpiece of condensation bath is connected by the inlet end of gas meter with tail gas neutralization pond.

First constant speed and constant pressure pump is provided with pressure transducer A, second constant speed and constant pressure pump is provided with pressure transducer B, backpressure pump is provided with pressure transducer C, the two ends of core holding unit are respectively arranged with pressure transducer D and pressure transducer E, automatic confined pressure is followed the trail of on pump and is provided with pressure transducer F, molten sulfur intermediate receptacle is provided with temperature sensor, constant temperature oven is provided with Thermostat Temperature Control instrument, high precision magnetic levitation balance is provided with magnetic suspension balance sensor, pressure transducer A, pressure transducer B, pressure transducer C, pressure transducer D, pressure transducer E, pressure transducer F, temperature sensor, Thermostat Temperature Control instrument, gas meter is connected with the data input pin of data acquisition board respectively with the data output end of magnetic suspension balance sensor, data acquisition board is also connected with computing machine and intercoms mutually.

Molten sulfur intermediate receptacle, water sample intermediate receptacle, gas sample intermediate receptacle, filtrator, core holding unit, conical flask and high temperature high voltage resistant gas-liquid separator are all arranged in constant temperature oven.

Described gas sample intermediate receptacle is also provided with emptying endpiece, and its emptying endpiece is connected with atmospheric valve.

Described is that gas sample intermediate receptacle, water sample intermediate receptacle and molten sulfur intermediate receptacle are piston container, the interior separation of piston container is two not connected cavitys, upper end cavity is connected with the endpiece of piston container, and lower end cavity is connected with the inlet end of piston container.

Described molten sulfur intermediate receptacle is the device for solid-state sulphur being molten into molten sulfur, and its arranged outside has ground heated filament heating arrangement, temperature sensor on this ground heated filament heating arrangement.

The outside of described constant temperature oven and condensation bath and tail gas neutralization pond is equipped with isolation tempered glass cover, and the upper end of this isolation tempered glass cover is also provided with hydrogen sulfide gas leakage warning device and explosion-proof exhaust fan.

The two ends of described core holding unit are parallel with differential pressure indicator.

High Temperature High Pressure acid gas reservoir gas-liquid sulphur phase percolation curve method of testing, it comprises following multiple step:

Step 1, rock core is chosen and process: choose representational rock core sample, according to corresponding standard, rock core sample is carried out extracting, cleaning, drying and processing, measures the length L of described rock core sample, diameter d, core porosity φ, permeability K after process.

Step 2, the saturated local water of rock core: according to rock core sample actual formation water data preparation simulated formation aqueous solution, at normal temperatures the local water prepared is filled water sample intermediate receptacle, utilize experimental provision to vacuumize process to rock core sample.

Open the liquid control valve of the operation valve of the second constant speed and constant pressure pump, the inlet end operation valve of water sample intermediate receptacle, the endpiece operation valve of water sample intermediate receptacle, the inlet end operation valve of core holding unit, the endpiece operation valve of core holding unit and high temperature high voltage resistant gas-liquid separator.

Close the gas control valve of the inlet end operation valve of molten sulfur intermediate receptacle, the operation valve of filtrator, the operation valve of gas sample intermediate receptacle, back pressure control valve, high temperature high voltage resistant gas-liquid separator.

Connecting filling the water sample intermediate receptacle of local water, core holding unit and high temperature high voltage resistant gas-liquid separator, opening the piston that the second constant speed and constant pressure pump promotes in water sample intermediate receptacle, by abundant for rock core sample saturated local water.

Step 3, Reality simulation stratum irreducible water condition: open the operation valve of nitrogen pot and the operation valve of gas supercharge pump, by gas boosting pump, nitrogen is filled gas sample intermediate receptacle at normal temperatures, then, closes the operation valve of nitrogen pot and the operation valve of gas supercharge pump.

Close the endpiece operation valve of water sample intermediate receptacle, the operation valve of filtrator and back pressure control valve.

Open the gas control valve of the operation valve of the first constant speed and constant pressure pump, the operation valve of gas sample intermediate receptacle, the inlet end operation valve of core holding unit, the endpiece operation valve of core holding unit, the liquid control valve of high temperature high voltage resistant gas-liquid separator and high temperature high voltage resistant gas-liquid separator.

Connect gas sample intermediate receptacle, core holding unit and the high temperature high voltage resistant gas-liquid separator of filling nitrogen, first follow the trail of pump by automatic confined pressure before displacement running and load certain confined pressure to core holding unit, open the piston in the first constant speed and constant pressure pump promotion gas sample intermediate receptacle, nitrogen flooding is made to replace local water in rock core sample, displace local water, until the liquid outlet end of high temperature high voltage resistant gas-liquid separator does not go out local water, displacement process terminates.

Step 4, molten sulfur prepares: the high sulfur-containing natural gas sample choosing actual acid gas reservoir, the atmospheric valve of gas sample intermediate receptacle is first opened before injecting sample gas, the remaining nitrogen of dropping a hint in sample intermediate receptacle, then close the atmospheric valve of sample intermediate receptacle of holding one's breath, under normal temperature, by gas boosting pump, gas sample intermediate receptacle is filled the high pressure sulfur-containing gas of reservoir pressure; According to actual gas reservoir sulfur component, choose corresponding solid-state sulphur, and put it into the molten sulfur intermediate receptacle of high temperature, by the mode of molten sulfur intermediate receptacle conducting self-heating, make solid-state sulphur reach fusing point fusing and form liquid sulfur.

Step 5, simulated formation high temperature and high pressure environment: follow the trail of pump by automatic confined pressure and load the simulation stratum condition confined pressure set to core holding unit; Utilize constant temperature oven simulated formation high temperature, and ensure to there will not be in whole molten sulfur displacement process solidification and blocking pipeline and rock core sample.

Step 6, determine the condition of the molten sulfur phase permeability under irreducible water saturation:

Open the gas control valve of the operation valve of the second constant speed and constant pressure pump, the inlet end operation valve of molten sulfur intermediate receptacle, the endpiece operation valve of molten sulfur intermediate receptacle, the operation valve of filtrator, the inlet end operation valve of core holding unit, the endpiece operation valve of core holding unit, the liquid control valve of high temperature high voltage resistant gas-liquid separator and high temperature high voltage resistant gas-liquid separator.

Close the inlet end operation valve of water sample intermediate receptacle, the endpiece operation valve of water sample intermediate receptacle, the operation valve of gas sample intermediate receptacle and back pressure control valve.

Connect molten sulfur intermediate receptacle, core holding unit and high temperature high voltage resistant gas-liquid separator that high temperature molten sulfur is housed; Open the piston in the second constant speed and constant pressure pump promotion molten sulfur intermediate receptacle, the rock core sample of the molten sulfur displacement irreducible water in molten sulfur intermediate receptacle.

Step 7: adopt the second constant speed and constant pressure pump to carry out the displacement of constant voltage molten sulfur, after the volume of voids that constant voltage displacement reaches 10 times, the pressure reduction imported and exported until core holding unit two ends and rate of discharge stable after, timing determines oral fluid sulphur flow, METHOD FOR CONTINUOUS DETERMINATION three molten sulfur phase permeabilities, its relative error is less than 3%, with this molten sulfur phase permeability K _s, as solution-air sulphur relative permeability basis; The computing formula of the molten sulfur phase permeability under irreducible water saturation is:

$K_S\left(S_{\mathrm{wi}}\right)=\frac{q_S{\mathrm{\μ}}_{S}L}{A(P_1-P_2)}{B}_S\×{10}^2$

In formula: K _s---molten sulfur phase effective permeability under irreducible water state, its unit is mD;

B _s---the molten sulfur volume factor under formation temperature, pressure condition;

Q _s---the flow of molten sulfur under rock core top hole pressure, its unit is mL/s;

μ _s---the viscosity of molten sulfur under formation temperature, pressure condition, its unit is mPas;

L---rock core sample length, its unit is cm;

A---rock core sample sectional area, its unit is cm ²;

P ₁---rock core sample intake pressure, its unit is MPa;

P ₂---rock core sample top hole pressure, its unit is MPa;

S _wi---rock core sample irreducible water saturation.

Step 8, what solution-air sulphur injected in setting ratio oozes test mutually, and it comprises following multiple sub-step:

Sub-step 1: open the operation valve of the first constant speed and constant pressure pump, the operation valve of the second constant speed and constant pressure pump, the inlet end operation valve of molten sulfur intermediate receptacle, the endpiece operation valve of molten sulfur intermediate receptacle, the operation valve of filtrator, the operation valve of gas sample intermediate receptacle, the inlet end operation valve of core holding unit, the endpiece operation valve of core holding unit, the liquid control valve of high temperature high voltage resistant gas-liquid separator, the gas control valve of high temperature high voltage resistant gas-liquid separator and back pressure control valve.

Close operation valve, the inlet end operation valve of water sample intermediate receptacle, the endpiece operation valve of water sample intermediate receptacle of gas boosting pump, connect gas sample intermediate receptacle, molten sulfur intermediate receptacle, core holding unit and the high temperature high voltage resistant gas-liquid separator of filling high sulfur-containing natural gas.

Sub-step 2: simultaneously start the first constant speed and constant pressure pump and the second constant speed and constant pressure pump, set constant speed or constant voltage, the endpiece of core holding unit sets back pressure, high sulfur-containing natural gas and molten sulfur are injected core holding unit with the ratio set, start solution-air sulphur and ooze test experiments mutually, the endpiece of core holding unit is by high temperature high voltage resistant gas-liquid separator, molten sulfur and gas are carried out gas-liquid separation, the endpiece of high temperature high voltage resistant gas-liquid separator gas is bathed through condensation, be mixed with water vapour in removing gas, measured the gas flow of condensation bath endpiece by gas meter; Molten sulfur flows into conical flask from the liquid outlet end of high temperature high voltage resistant gas-liquid separator, and this conical flask is in suspended state under hanging on high precision magnetic levitation balance, measures not molten sulfur quality in the same time, calculate corresponding molten sulfur amount by high precision magnetic levitation balance.

Sub-step 3: after experiment is less than 0.005 to high sulfur-containing natural gas phase effective permeability permeability, measures molten sulfur phase effective permeability and terminates experiment.

Step 9, record accumulation production fluid sulfur content V _siwith tolerance V _giand carry out formation condition correction: the inlet and outlet pressure P recording the different injection ratio rock core two ends of two kinds of fluids ₁, P ₂accumulation production fluid sulfur content V under the top hole pressure condition of differential pressure Δ P and rock clamper _siwith tolerance V _gi.

By the volume factor of corresponding formation condition fluid surface condition semi-invariant changed into the amount under formation condition, its computing formula related to is:

V' _Si＝V _SiB _S

V' _gi＝(V _gi-V _SiR _SG)B _G

In formula: V' _si---accumulation production fluid sulfur content under two kinds of fluid a certain injection ratio formation conditions after correction, its unit is cm ³;

V' _gi---cumulative gas production under two kinds of fluid a certain injection ratio formation conditions after correction, its unit is cm ³;

V _si---accumulation production fluid sulfur content under two kinds of fluid a certain injection ratio formation conditions, its unit is cm ³;

V _gi---cumulative gas production under two kinds of fluid a certain injection ratio formation conditions, its unit is cm ³;

R _sG---the original solution gas liquor ratio of molten sulfur;

B _s---molten sulfur initial volume coefficient;

B _g---high sulfur-containing natural gas initial volume coefficient;

Wherein, the original solution gas liquor ratio R of molten sulfur _sGwith molten sulfur initial volume coefficient B _smeasured by PVT tester, its computing formula is:

$R_{\mathrm{SG}}=\frac{V_G{\mathrm{\ρ}}_S}{W_S}$

$B_S=\frac{V_S{\mathrm{\ρ}}_S}{W_S}$

In formula: W _s---the quality of degassed molten sulfur, its unit is g;

ρ _s---the density of degassed molten sulfur under surface temperature, its unit is g/cm ³;

V _g---the volume in molten sulfur under the isolated status of criterion, its unit is cm ³;

V _s---release the subsurface volume of molten sulfur, its unit is cm ³;

Wherein, high sulfur-containing natural gas initial volume coefficient B _gcomputing formula be:

$B_G=Z\frac{273+T}{293}\frac{P_{\mathrm{SC}}}{P}$

In formula: Z---high sulfur-containing natural gas formation condition Z-factor;

T---formation temperature, its unit is DEG C;

P---reservoir pressure, its unit is MPa;

P _sC---surface air pressure, its unit is MPa.

Step 10, calculates the molten sulfur phase relative permeability K in each moment _rs, gas phase relative permeability K _rgwith core sample gas saturation S _g:

1. the gas phase effective permeability K in each moment _gcomputing formula be:

In formula, K _g---gas phase effective permeability, its unit is mD;

A---the sectional area of rock core sample, its unit is cm ²;

P _a---atmospheric pressure, its unit is MPa;

L---the length of rock core sample, its unit is cm;

Q _g---the high sulfur-containing natural gas flow at reservoir pressure, temperature, its unit is cm ³/ s;

P ₁---the pressure of core holding unit inlet end, its unit is MPa;

P ₂---the pressure of outlet port of rock core holder, its unit is MPa;

μ _g---high sulfur-containing natural gas viscosity under formation condition, its unit is mPas.

2. the liquid phase effective permeability K in each moment _scomputing formula be:

In formula, K _s---liquid phase effective permeability, its unit is mD;

μ _s---molten sulfur viscosity under formation condition, its unit is mPas;

Q _s---the molten sulfur flow at reservoir pressure, temperature, its unit is cm ³/ s.

3. the gas phase relative permeability K in each moment _rgcomputing formula be:

$K_{\mathrm{rg}}=\frac{K_g}{K_S\left(S_{\mathrm{wi}}\right)}$

In formula, K _rg---gas phase relative permeability;

S _wi---rock core sample irreducible water saturation.

4. the molten sulfur phase relative permeability K in each moment _rScomputing formula be:

$K_{\mathrm{rS}}=\frac{K_S}{K_S\left(S_{\mathrm{wi}}\right)}.$

5. the rock core sample exit end face in each moment is containing molten sulfur saturation degree S _scomputing formula be:

$S_S=\frac{{V^{\′}}_{\mathrm{Si}}-V_{S0}}{V_P}$

In formula, V _s0---the volume of original measurement container molten sulfur, its unit is cm ³;

V _p---rock core sample volume of voids, its unit is cm ³.

6. the rock core sample exit end face gas saturation S in each moment _gcomputing formula be:

S _g＝1-S _wi-S _S。

Solution-air sulphur in described sub-step 2 oozes in test experiments mutually, when each injection is to the high sulfur-containing natural gas of certainty ratio and molten sulfur, the injection rate IR of often kind of fluid is at least 3 times of rock core sample volume of voids, and after the pressure at two ends of core holding unit is stable, then record experimental data.

Parameter high sulfur-containing natural gas formation condition Z-factor Z described in step 9 is obtained by Dranchuk-Abu-Kassem experimental formula computing method, and its computing formula is:

$\begin{array}{c}1+(A_1+\frac{A_2}{T_{\mathrm{pr}}}+\frac{A_3}{T_{\mathrm{pr}}^3}+\frac{A_4}{T_{\mathrm{pr}}^4}+\frac{A_5}{T_{\mathrm{pr}}^5}){\mathrm{\ρ}}_r+(A_6+\frac{A_7}{T_{\mathrm{pr}}}+\frac{A_8}{T_{\mathrm{pr}}^2}){\mathrm{\ρ}}_r^2-\\ A_9(\frac{A_7}{T_{\mathrm{pr}}}+\frac{A_8}{T_{\mathrm{pr}}^2}){\mathrm{\ρ}}_r^5+\frac{A_{10}}{T_{\mathrm{pr}}^3}{\mathrm{\ρ}}_r^2(1+A_{11}{\mathrm{\ρ}}_r^2)\exp (-A_{11}{\mathrm{\ρ}}_r^2)-0.27\frac{p_{\mathrm{pr}}}{{\mathrm{\ρ}}_r{T}_{\mathrm{pr}}}=0\end{array}$

$\begin{array}{c}Z=1+(A_1+\frac{A_2}{T_{\mathrm{pr}}}+\frac{A_3}{T_{\mathrm{pr}}^3}){\mathrm{\ρ}}_r+(A_4+\frac{A_5}{T_{\mathrm{pr}}}){\mathrm{\ρ}}_r^2+\left(\frac{A_5{A}_6}{T_{\mathrm{pr}}}\right){\mathrm{\ρ}}_r^5\\ +\frac{A_7}{T_{\mathrm{pr}}^3}{\mathrm{\ρ}}_r^2(1+A_8{\mathrm{\ρ}}_r^2)\exp \left({-A}_8{\mathrm{\ρ}}_r^2\right)\end{array}$

In formula, coefficient A ₁~ A ₁₁value be: A ₁=0.3265, A ₂=-1.07, A ₃=-0.5339, A ₄=0.01569, A ₅=-0.05165, A ₆=0.5475, A ₇=-0.7361, A ₈=0.1844, A ₉=0.1056, A ₁₀=0.6134, A ₁₁=0.721.

Work as T _prspan be 1.0≤T _prwhen≤3, p _prspan be 0.2≤p _pr≤ 30.

Work as T _prspan be 0.7≤T _prwhen≤1.0, p _prspan be p _pr<1.0.

Molten sulfur viscosity, mu under formation condition described in step 10 _scalculated by liquid sulfur viscosity experimental formula, its computing formula is:

${\mathrm{\&mu;}}_S=\left\{\begin{array}{cc}0.45271-2.0357\&times;{10}^{-3}T+2.3208\&times;{10}^{-6}{T}^2,& 392.1K<T<433.2K\\ 392350-2660.9T+6.0061T^2-4.5115\&times;{10}^{-3}{T}^3,& 433.2K<T<463.2K\\ \frac{108.03}{{(1+e^{0.0816(T-476.08)})}^{0.512}}+0.9423,& Y>463.2K\end{array}\right.$

In formula, μ _s---liquid sulfur viscosity, its unit is mPas;

T---temperature, its unit is K.

High sulfur-containing natural gas viscosity, mu under formation condition described in step 10 _g, calculated by Dempsey empirical formula method, its computing formula is:

$\begin{array}{c}\ln \left(\frac{{\mathrm{\&mu;}}_g{T}_r}{{\mathrm{\&mu;}}_1}\right)=A_0+A_1{p}_r+A_2{p}_r^2+A_3{p}_r^3+T_r(A_4+A_5{p}_r+A_6{p}_r^2+A_7{p}_r^3)\\ +T_r^2(A_8+A_9{p}_r+A_{10}{p}_r^2+A_{11}{p}_r^3)+T_r^3(A_{12}+A_{13}p+A_{14}{p}_r^2+A_{15}{p}_r^3)\\ {\mathrm{\&mu;}}_1=(1.709\&times;{10}^{-5}-2.062\&times;{10}^{-6}{\mathrm{\&gamma;}}_g)(1.8T+32)+8.188\&times;{10}^{-3}\\ -6.15\&times;{10}^{-3}\lg \left({\mathrm{\&gamma;}}_g\right)\end{array}$

In formula, parameter A ₀~ A ₁₅value be: A ₀=-2.4621182, A ₁=2.97054714, A ₂=-0.286264054, A ₃=0.00805420522, A ₄=2.80860949, A ₅=-3.49803305, A ₆=0.36037302, A ₇=-0.0104432413, A ₈=-0.793385684, A ₉=1.39643306, A ₁₀=-0.149144925, A ₁₁=0.00441015512, A ₁₂=0.0839387178, A ₁₃=-0.186408846, A ₁₄=0.0203367881, A ₁₅=-0.000609579263;

μ ₁---to place an order component gas viscosity at 1 atmospheric pressure with to fixed temperature, its unit is mPas;

γ _g---the relative density of high sulfur-containing natural gas.

The invention has the beneficial effects as follows: the present invention proposes a kind of the High Temperature High Pressure solution-air sulphur phase percolation curve proving installation and the method that meet acid gas reservoir Development and Production reality, this method of testing can measure High Temperature High Pressure solution-air sulphur safe, convenient, fast, accurately and efficiently and ooze data mutually, for acid gas reservoir formulates the Data support that rational development plan provides science.

Present invention achieves formation condition High Temperature High Pressure acid gas reservoir solution-air sulphur and ooze experiment mutually, magnetic suspension balance is adopted to measure high-precision measuring phase sepage sulfur content, realize experiment overall process real time data acquisition simultaneously, fill up the blank that solution-air sulphur oozes experiment mutually, this experiment more can measure molten sulfur in precise and safety ground, high sulfur-containing natural gas phase milliosmolarity, and with experimental formula, laboratory experiment is measured fluid-phase milliosmolarity by experiment and be modified to formation condition fluid-phase milliosmolarity, test result is made more to meet stratum reality, experimental data is more reliable, for acid gas reservoir formulates the Data support that efficient and rational development plan provides science, also to have security good for this proving installation simultaneously, precision is high, the advantage such as convenient to operation.

Accompanying drawing explanation

Fig. 1 is the structure principle chart of the High Temperature High Pressure solution-air sulphur phase percolation curve proving installation of acid gas reservoir Development and Production reality of the present invention;

Fig. 2 is the structure principle chart of high precision magnetic levitation balance in proving installation of the present invention;

Fig. 3 is the system principle diagram of data acquisition system (DAS) in proving installation of the present invention;

Fig. 4 is the process flow diagram of the High Temperature High Pressure solution-air sulphur phase percolation curve method of testing of acid gas reservoir Development and Production reality of the present invention;

In figure, 1-sulfur-containing gas sample pot, 2-nitrogen pot, 3-nitrogen pot operation valve, 4-sample pot operation valve, 5-gas boosting pump, 6-gas boosting pump control valve, 7-gas sample intermediate receptacle atmospheric valve, 8-gas sample intermediate receptacle, 9-gas sample intermediate receptacle operation valve, 10-pressure transducer A, 11-first constant speed and constant pressure pump control valve, 12-first constant speed and constant pressure pump, 13-temperature sensor, 14-molten sulfur intermediate receptacle, 15-molten sulfur intermediate receptacle discharge control valve, 16-filtrator, 17-filtrator operation valve, 18-pressure transducer B, 19-second constant speed and constant pressure pump, 20-second constant speed and constant pressure pump control valve, 21-molten sulfur intermediate receptacle inlet control valve, 22-water sample intermediate receptacle, 23-water sample intermediate receptacle inlet control valve, 24-Thermostat Temperature Control instrument, 25-constant temperature oven, 26-core holding unit inlet control valve, 27-core holding unit, 28-differential pressure indicator, 29-pressure transducer C, 30-back pressure control valve, 31-backpressure pump, 32-high precision magnetic levitation balance, 33-high temperature high voltage resistant gas-liquid separator gas control valve, 34-condensation is bathed, 35-gas meter, 36-tail gas neutralization pond, 37-water sample intermediate receptacle discharge control valve, 38-pressure transducer D, the automatic confined pressure of 39-follows the trail of pump control valve, 40-pressure transducer E.41-high temperature high voltage resistant gas-liquid separator liquid control valve, 42-high temperature high voltage resistant gas-liquid separator, 43-core holding unit discharge control valve, 44-conical flask, 45-pressure transducer F, the automatic confined pressure of 46-follows the trail of pump, 47-magnetic suspension balance sensor, 48-electromagnet, 49-alnico magnets, 50-data acquisition board, 51-computing machine.

Embodiment

Below in conjunction with accompanying drawing, technical scheme of the present invention is described in further detail, but protection scope of the present invention is not limited to the following stated.

(1) High Temperature High Pressure acid gas reservoir gas-liquid sulphur phase percolation curve proving installation

As shown in Figure 1, a kind of High Temperature High Pressure acid gas reservoir gas-liquid sulphur phase percolation curve proving installation, it comprises displacement system, formation condition simulation system, back pressure system, data testing system and data acquisition system (DAS).

(1) displacement system

Described displacement system comprises sulfur-containing gas sample pot 1, nitrogen pot 2, gas boosting pump 5, gas sample intermediate receptacle 8, first constant speed and constant pressure pump 12, molten sulfur intermediate receptacle 14, water sample intermediate receptacle 22, second constant speed and constant pressure pump 19, filtrator 16;

The endpiece of described first constant speed and constant pressure pump 12 is communicated with by the inlet end of pipeline with gas sample intermediate receptacle 8, this pipeline is arranged on the first constant speed and constant pressure pump control valve 11, first constant speed and constant pressure pump 12 and arranges pressure transducer A10.

The endpiece of gas sample intermediate receptacle 8 is communicated with the endpiece of gas boosting pump 5 with gas supercharge pump operation valve 6 by pipeline, the endpiece of gas sample intermediate receptacle 8 is also communicated with the inlet end of core holding unit 27 with core holding unit inlet end operation valve 26 by gas sample intermediate receptacle operation valve 9 successively, and the emptying endpiece of gas sample intermediate receptacle 8 is also provided with gas sample intermediate receptacle atmospheric valve 7.

The inlet end of gas boosting pump 5 is connected with the endpiece of sample pot operation valve 4 with nitrogen pot 2 and sulfur-containing gas sample pot 1 respectively by nitrogen pot operation valve 3.

The endpiece of the second constant speed and constant pressure pump 19 is communicated with the inlet end of water sample intermediate receptacle 22 with water sample intermediate receptacle inlet control valve 23 by the second constant speed and constant pressure pump control valve 20 successively, the endpiece of the second constant speed and constant pressure pump 19 is also communicated with the inlet end of molten sulfur intermediate receptacle 14 with molten sulfur intermediate receptacle inlet control valve 21 by the second constant speed and constant pressure pump control valve 20 successively, and the second constant speed and constant pressure pump 19 arranges pressure transducer B18.

Water sample intermediate receptacle 22 endpiece is communicated with the inlet end of core holding unit 27 with core holding unit inlet end operation valve 26 by water sample intermediate receptacle discharge control valve 37 successively.

The endpiece of molten sulfur intermediate receptacle 14 arranges molten sulfur intermediate receptacle discharge control valve 15, is connected with molten sulfur intermediate receptacle discharge control valve 15 by pipeline with filtrator 16.The endpiece of filtrator 16 is provided with filtrator operation valve 17, is communicated with core holding unit inlet end operation valve 26 by filtrator operation valve 17 with the inlet end of core holding unit 27.

Gas sample intermediate receptacle 8 and water sample intermediate receptacle 22 are piston container, and be disconnected two cavitys mutually by the interior separation of this piston container by piston, upper end cavity stored sample, lower end cavity connects constant speed and constant pressure pump.Gas sample intermediate receptacle 8 and water sample intermediate receptacle 22 are respectively used to deposit high sulfur-containing natural gas gas sample and local water, drive the piston of its inside respectively by the first constant speed and constant pressure pump 12 and the second constant speed and constant pressure pump 19, will the high-hydrogen sulfide gas sample of gas sample intermediate receptacle 8 is placed in and be placed in the local water displacement of water sample intermediate receptacle 22 to core holding unit 27.

First constant speed and constant pressure pump 12 and the second constant speed and constant pressure pump 19 are for providing the continuous no pulse displacement of fluid, energy constant speed, constant voltage work, its maximum working pressure (MOP) all can be: 120MPa, constant speed scope: 0.00001 ~ 16ml/min, flow accuracy: 0.5%, pressure precision: 0.1%FS.

Gas boosting pump 5 can for the gaseous sample supercharging in gas sample intermediate receptacle 8 be to reach required formation condition;

Molten sulfur intermediate receptacle 14 is piston container, it is a kind of device for solid-state sulphur being molten into molten sulfur, this piston container is outer with underground heat silk heating arrangement, the temperatures as high 200 DEG C of this molten sulfur intermediate receptacle 14 can be made, and its efficiency of heating surface is high, ground heated filament heating arrangement is provided with temperature sensor 13, the temperature of Real-Time Monitoring molten sulfur intermediate receptacle 14.

Filtrator 16 can filter the solid particulate matter in molten sulfur, prevents solid particulate matter blocking pipeline and core sample.

(2) formation condition simulation system

Described formation condition simulation system comprises the constant temperature oven 25 for simulated formation temperature, the automatic confined pressure for simulated formation pressure follows the trail of pump 46 and core holding unit 27.

The inlet/outlet two ends of core holding unit 27 are respectively equipped with core holding unit inlet control valve 26 and core holding unit discharge control valve 43, its inlet end is also provided with pressure transducer D38, endpiece is also provided with pressure transducer E40, core holding unit discharge control valve 43 connects high temperature high voltage resistant gas-liquid separator 42 and back pressure control valve 30 respectively by pipeline, automatic confined pressure is followed the trail of pump 46 and is connected core holding unit 27, this pipeline is provided with automatic confined pressure and follows the trail of pump control valve 39, and automatic confined pressure is followed the trail of pump 46 and arranged pressure transducer F45.

Molten sulfur intermediate receptacle 14, water sample intermediate receptacle 22, gas sample intermediate receptacle 8, filtrator 16, core holding unit 27, conical flask 44, high temperature high voltage resistant gas-liquid separator 42 and corresponding connecting line all must be placed in constant temperature oven 25.

Automatic confined pressure is followed the trail of pump 46 and is adopted hydraulic way to load stratum confined pressure to core holding unit 27, by pressure transducer D38, pressure transducer E40 and its internal pressure of pressure transducer F45 real-time tracing, and internal pressure can not change with the gradient of temperature of core holding unit 27.

Core holding unit 27 adopts the Hastelloy material of sulfur resistive to make, and high temperature high voltage resistant is lightweight, for the mensuration of solution-air sulphur phase permeability.

Constant temperature oven 25 is for simulated formation temperature conditions, and the middle part of constant temperature oven 25 is provided with temperature controller 24, can Real-Time Monitoring with control the temperature of constant temperature oven 25, temperature controlling range: room temperature ~ 180 DEG C, temperature precise control: ± 0.5 DEG C;

(3) back pressure system

Described back pressure system comprises back pressure control valve 30, manual backpressure pump 31 and pressure transducer C29, one end of back pressure control valve 30 is communicated with the endpiece of core holding unit 27 by core holding unit discharge control valve 43, the other end is connected with manual backpressure pump 31, manual backpressure pump is arranged pressure transducer C29.

Back pressure control valve 30 is for regulating pressure size and the stability of core holding unit 27 endpiece.

Manual backpressure pump 31 is the endpiece on-load pressure of core holding unit 27 by the mode of hydraulic pressure, and this manual backpressure pump 31 arranges pressure transducer C29.

(4) data testing system

Described data testing system comprises high precision magnetic levitation balance 32, high temperature high voltage resistant gas-liquid separator 42, conical flask 44, condensation bath 34, gas meter 35 and tail gas neutralization pond 36.

The inlet end of high temperature high voltage resistant gas-liquid separator 42 is connected by the endpiece of core holding unit discharge control valve 43 with core holding unit 27; The inlet end that the gas outlet end of high temperature high voltage resistant gas-liquid separator 42 bathes 34 by high temperature high voltage resistant gas-liquid separator gas control valve 33 and condensation is connected, and the endpiece of condensation bath 34 is connected with tail gas neutralization pond 36 by gas meter 35; The liquid outlet end of high temperature high voltage resistant gas-liquid separator 42 is connected by the inlet end of high temperature high voltage resistant gas-liquid separator liquid control valve 41 with conical flask 44.

As shown in Figure 2, conical flask 44 hangs on high precision magnetic levitation balance 32, the hook top of conical flask 44 is provided with alnico magnets 49, electromagnet 48 is provided with bottom the hanging stick of high precision magnetic levitation balance 32, make conical flask 44 be in suspended state by these alnico magnets 49 and electromagnet 48, the quality of high temperature molten sulfur in conical flask 44 measured in real time by high precision magnetic levitation balance 32.High precision magnetic levitation balance 32 is also provided with magnetic suspension balance sensor 47.

The performance index of high precision magnetic levitation balance 32 are: measuring accuracy: 0.01mg ~ 1ug, repeatability: ± 0.02mg ~ ± 2ug, can measure the slight change of mass of object under High Temperature High Pressure height Sulphur Contaminated Environment.High precision magnetic levitation balance 32 is for measuring the quality of molten sulfur in conical flask 44 in real time, and measuring accuracy is high.

The effect of high temperature high voltage resistant gas-liquid separator 42 is the molten sulfur and gas separaion that are exported by core holding unit 27, is convenient to the measurement of both flows.

Condensation bath 34 can select liquid nitrogen condensation to bathe, and the water vapour that the gas outlet end for condensation high temperature high voltage resistant gas-liquid separator 42 exports reduces measuring gas flow rate error.

Gas meter 35 is for measuring rock sample endpiece gas flow.

Tail gas neutralization pond 36 can select NaOH solution neutralization pond, for carrying out neutralisation treatment to experiment tail gas, preventing hydrogen sulfide gas from directly entering atmospheric environment, and causing dangerous accident to occur.

(5) data acquisition system (DAS)

As shown in Figure 3, described data acquisition system (DAS) comprises pressure transducer A10, pressure transducer B18, pressure transducer C29, pressure transducer D38, pressure transducer E40, pressure transducer F45, temperature sensor 13, Thermostat Temperature Control instrument 24, gas meter 35, magnetic suspension balance sensor 47, data acquisition board 50 and computing machine 51.

The probe of pressure transducer A10 is placed on the first constant speed and constant pressure pump 12, the probe of pressure transducer B18 is placed on the second constant speed and constant pressure pump 19, the probe of pressure transducer C29 is placed on manual backpressure pump 31, the probe of pressure transducer D38, pressure transducer E40 is placed in the two ends of core holding unit 27 respectively, the probe of pressure transducer F45 is placed in automatic confined pressure and follows the trail of on pump 46, the probe of temperature sensor 13 is placed on molten sulfur intermediate receptacle 14, and Thermostat Temperature Control instrument 24 is placed in the middle part of constant temperature oven 25.

Pressure transducer A10, pressure transducer B18, pressure transducer C29, pressure transducer D38, pressure transducer E40, pressure transducer F45, temperature sensor 13, Thermostat Temperature Control instrument 24, the output terminal of all the sensors such as gas meter 35 and magnetic suspension balance sensor 47 connects with the Gather and input end of data acquisition board 50 respectively, data acquisition board 50 will collect data and output to computing machine 51, by computing machine 51, its data are carried out to the analyzing and processing in later stage, also can carry out control adjustment according to the data collected to the temperature of Thermostat Temperature Control instrument 24.

Described pressure transducer, temperature sensor 13, gas meter 35 and magnetic suspension balance sensor 47 are all for being real-time transmitted to data acquisition board 50 by corresponding signal, experimental data is transferred to computing machine 51 by data acquisition board 50, uses software to carry out respective handling to experimental data.

Constant temperature oven 25 involved in the present invention, condensation bath 34 and tail gas neutralization pond 36, be equipped with isolation tempered glass cover, and arrange hydrogen sulfide gas leakage warning device and explosion-proof exhaust fan in the upper end of this isolation tempered glass cover outside it.Because hydrogen sulfide gas has severe toxicity, so the present invention need carry out safety prevention measure to whole experimental situation.

In order to improve resistance to corrosion, all pipelines, devices contacted with molten sulfur with high sulfur-containing gas all adopt the Hastelloy material of sulfur resistive.

(2) High Temperature High Pressure acid gas reservoir gas-liquid sulphur phase percolation curve method of testing

As shown in Figure 4, High Temperature High Pressure acid gas reservoir gas-liquid sulphur phase percolation curve method of testing, it comprises following multiple step:

(1) rock core is chosen and process

Choose representational rock core sample, be drilled to the cylinder that diameter is 2.50cm or 3.80cm, length is not less than 1.5 times of diameter, according to corresponding standard, rock core sample is carried out extracting, cleaning, drying and processing, after process, measure the length L of described rock core sample, diameter d, core porosity φ, permeability K.

(2) the saturated local water of rock core

According to rock core sample actual formation water data preparation simulated formation aqueous solution, at normal temperatures the local water prepared is filled water sample intermediate receptacle 22, utilize experimental provision to vacuumize process to rock core sample.

Open the liquid control valve of the operation valve of the second constant speed and constant pressure pump 19, the inlet end operation valve of water sample intermediate receptacle 22, the endpiece operation valve of water sample intermediate receptacle 22, the inlet end operation valve of core holding unit 27, the endpiece operation valve of core holding unit 27 and high temperature high voltage resistant gas-liquid separator 42.

Close the gas control valve of the inlet end operation valve of molten sulfur intermediate receptacle 14, the operation valve of filtrator 16, the operation valve of gas sample intermediate receptacle 8, back pressure control valve 30, high temperature high voltage resistant gas-liquid separator 42.

Connecting filling the water sample intermediate receptacle 22 of local water, core holding unit 27 and high temperature high voltage resistant gas-liquid separator 42, opening the piston that the second constant speed and constant pressure pump 19 promotes in water sample intermediate receptacle 22, by abundant for rock core sample saturated local water.

(3) Reality simulation stratum irreducible water condition

Open the operation valve of nitrogen pot 2 and the operation valve of gas supercharge pump 5, by gas boosting pump 5, nitrogen is filled gas sample intermediate receptacle 8 at normal temperatures, then, close the operation valve of nitrogen pot 2 and the operation valve of gas supercharge pump 5.

Close the endpiece operation valve of water sample intermediate receptacle 22, the operation valve of filtrator 16 and back pressure control valve 30.

Open the gas control valve of the operation valve of the first constant speed and constant pressure pump 12, the operation valve of gas sample intermediate receptacle 8, the inlet end operation valve of core holding unit 27, the endpiece operation valve of core holding unit 27, the liquid control valve of high temperature high voltage resistant gas-liquid separator 42 and high temperature high voltage resistant gas-liquid separator 42.

Connect gas sample intermediate receptacle 8, core holding unit 27 and the high temperature high voltage resistant gas-liquid separator 42 of filling nitrogen, first follow the trail of pump 46 by automatic confined pressure before displacement running and load certain confined pressure to core holding unit 27, open the piston that the first constant speed and constant pressure pump 12 promotes in gas sample intermediate receptacle 8, nitrogen flooding is made to replace local water in rock core sample, displace local water, until the liquid outlet end of high temperature high voltage resistant gas-liquid separator 42 does not go out local water, displacement process terminates.

(4) molten sulfur prepares

Choose the high sulfur-containing natural gas sample of actual acid gas reservoir, the atmospheric valve of gas sample intermediate receptacle 8 is first opened before injecting sample gas, the remaining nitrogen of dropping a hint in sample intermediate receptacle 8, then close the atmospheric valve of sample intermediate receptacle 8 of holding one's breath, under normal temperature, by gas boosting pump 5, gas sample intermediate receptacle 8 is filled the high pressure sulfur-containing gas of reservoir pressure; According to actual gas reservoir sulfur component, choose corresponding solid-state sulphur, and put it into the molten sulfur intermediate receptacle 14 of high temperature, by the mode of molten sulfur intermediate receptacle 14 conducting self-heating, make solid-state sulphur reach fusing point fusing and form liquid sulfur.

(5) simulated formation high temperature and high pressure environment

Follow the trail of pump 46 by automatic confined pressure and load the simulation stratum condition confined pressure set to core holding unit 27; Utilize constant temperature oven 25 simulated formation high temperature, and ensure to there will not be in whole molten sulfur displacement process solidification and blocking pipeline and rock core sample.

(6) condition of the molten sulfur phase permeability under irreducible water saturation is determined:

Open the gas control valve of the operation valve of the second constant speed and constant pressure pump 19, the inlet end operation valve of molten sulfur intermediate receptacle 14, the endpiece operation valve of molten sulfur intermediate receptacle 14, the operation valve of filtrator 16, the inlet end operation valve of core holding unit 27, the endpiece operation valve of core holding unit 27, the liquid control valve of high temperature high voltage resistant gas-liquid separator 42 and high temperature high voltage resistant gas-liquid separator 42.

Close the inlet end operation valve of water sample intermediate receptacle 22, the endpiece operation valve of water sample intermediate receptacle 22, the operation valve of gas sample intermediate receptacle 8 and back pressure control valve 30.

Connect molten sulfur intermediate receptacle 14, core holding unit 27 and high temperature high voltage resistant gas-liquid separator 42 that high temperature molten sulfur is housed; Open the piston that the second constant speed and constant pressure pump 19 promotes in molten sulfur intermediate receptacle 14, the rock core sample of the molten sulfur displacement irreducible water in molten sulfur intermediate receptacle 14.

(7) the molten sulfur phase permeability under irreducible water saturation is calculated

The second constant speed and constant pressure pump 19 is adopted to carry out the displacement of constant voltage molten sulfur, after the volume of voids that constant voltage displacement reaches 10 times, the pressure reduction imported and exported until core holding unit 27 two ends and rate of discharge stable after, timing determines oral fluid sulphur flow, METHOD FOR CONTINUOUS DETERMINATION three molten sulfur phase permeabilities, its relative error is less than 3%, with this molten sulfur phase permeability K _s, as solution-air sulphur relative permeability basis; The computing formula of the molten sulfur phase permeability under irreducible water saturation is:

$K_S\left(S_{\mathrm{wi}}\right)=\frac{q_S{\mathrm{\&mu;}}_{S}L}{A(P_1-P_2)}{B}_S\&times;{10}^2$

In formula: K _s---molten sulfur phase effective permeability under irreducible water state, its unit is mD;

B _s---the molten sulfur volume factor under formation temperature, pressure condition;

Q _s---the flow of molten sulfur under rock core top hole pressure, its unit is mL/s;

μ _s---the viscosity of molten sulfur under formation temperature, pressure condition, its unit is mPas;

L---rock core sample length, its unit is cm;

A---rock core sample sectional area, its unit is cm ²;

P ₁---rock core sample intake pressure, its unit is MPa;

P ₂---rock core sample top hole pressure, its unit is MPa;

S _wi---rock core sample irreducible water saturation.

(8) what solution-air sulphur injected in setting ratio oozes test mutually

The test of oozing mutually that solution-air sulphur injects in setting ratio comprises following multiple sub-step:

1, open the operation valve of the first constant speed and constant pressure pump 12, the operation valve of the second constant speed and constant pressure pump 19, the inlet end operation valve of molten sulfur intermediate receptacle 14, the endpiece operation valve of molten sulfur intermediate receptacle 14, the operation valve of filtrator 16, the operation valve of gas sample intermediate receptacle 8, the inlet end operation valve of core holding unit 27, the endpiece operation valve of core holding unit 27, the liquid control valve of high temperature high voltage resistant gas-liquid separator 42, the gas control valve of high temperature high voltage resistant gas-liquid separator 42 and back pressure control valve 30.

Close operation valve, the inlet end operation valve of water sample intermediate receptacle 22, the endpiece operation valve of water sample intermediate receptacle 22 of gas boosting pump 5, connect water sample intermediate receptacle 22, molten sulfur intermediate receptacle 14, core holding unit 27 and the high temperature high voltage resistant gas-liquid separator 42 of filling high sulfur-containing natural gas.

2, start the first constant speed and constant pressure pump 12 and the second constant speed and constant pressure pump 19 simultaneously, set constant speed or constant voltage, the endpiece of core holding unit 27 sets back pressure, high sulfur-containing natural gas and molten sulfur are injected core holding unit 27 with the ratio set, start solution-air sulphur and ooze test experiments mutually, the endpiece of core holding unit 27 is by high temperature high voltage resistant gas-liquid separator 42, molten sulfur and gas are carried out gas-liquid separation, the endpiece of high temperature high voltage resistant gas-liquid separator gas 42 is through condensation bath 34, water vapour is mixed with in removing gas, the gas flow that 34 endpiece are bathed in condensation is measured by gas meter 35, molten sulfur flows into conical flask 44 from the liquid outlet end of high temperature high voltage resistant gas-liquid separator 42, this conical flask 44 hangs on high precision magnetic levitation balance 32 times, be in suspended state, measure not molten sulfur quality in the same time by high precision magnetic levitation balance 32, calculate corresponding molten sulfur amount.

3, after experiment is less than 0.005 to high sulfur-containing natural gas phase effective permeability permeability, measures molten sulfur phase effective permeability and terminate experiment.

(9) accumulation production fluid sulfur content V is recorded _siwith tolerance V _giand carry out formation condition correction

Record the inlet and outlet pressure P at the different injection ratio rock core two ends of two kinds of fluids ₁, P ₂accumulation production fluid sulfur content V under the top hole pressure condition of differential pressure Δ P and rock clamper _siwith tolerance V _gi.

By the volume factor of corresponding formation condition fluid surface condition semi-invariant changed into the amount under formation condition, its computing formula related to is:

V' _Si＝V _SiB _S

V' _gi＝(V _gi-V _SiR _SG)B _G

In formula: V' _si---accumulation production fluid sulfur content under two kinds of fluid a certain injection ratio formation conditions after correction, its unit is cm ³;

V' _gi---cumulative gas production under two kinds of fluid a certain injection ratio formation conditions after correction, its unit is cm ³;

V _si---accumulation production fluid sulfur content under two kinds of fluid a certain injection ratio formation conditions, its unit is cm ³;

V _gi---cumulative gas production under two kinds of fluid a certain injection ratio formation conditions, its unit is cm ³;

R _sG---the original solution gas liquor ratio of molten sulfur;

B _s---molten sulfur initial volume coefficient;

B _g---high sulfur-containing natural gas initial volume coefficient.

Wherein, the original solution gas liquor ratio R of molten sulfur _sGwith molten sulfur initial volume coefficient B _smeasured by PVT tester, its computing formula is:

$R_{\mathrm{SG}}=\frac{V_G{\mathrm{\&rho;}}_S}{W_S}$

$B_S=\frac{V_S{\mathrm{\&rho;}}_S}{W_S}$

In formula: W _s---the quality of degassed molten sulfur, its unit is g;

ρ _s---the density of degassed molten sulfur under surface temperature, its unit is g/cm ³;

V _g---the volume in molten sulfur under the isolated status of criterion, its unit is cm ³;

V _s---release the subsurface volume of molten sulfur, its unit is cm ³.

Wherein, high sulfur-containing natural gas initial volume coefficient B _gcomputing formula be:

$B_G=Z\frac{273+T}{293}\frac{P_{\mathrm{SC}}}{P}$

In formula: Z---high sulfur-containing natural gas formation condition Z-factor;

T---formation temperature, its unit is DEG C;

P---reservoir pressure, its unit is MPa;

P _sC---surface air pressure, its unit is MPa.

(10) the molten sulfur phase relative permeability K in each moment is calculated _rs, gas phase relative permeability K _rgwith core sample gas saturation S _g

1, the gas phase effective permeability K in each moment _gcomputing formula be:

In formula, K _g---gas phase effective permeability, its unit is mD;

A---the sectional area of rock core sample, its unit is cm ²;

P _a---atmospheric pressure, its unit is MPa;

L---the length of rock core sample, its unit is cm;

Q _g---the high sulfur-containing natural gas flow at reservoir pressure, temperature, its unit is cm ³/ s;

P ₁---the pressure of core holding unit inlet end, its unit is MPa;

P ₂---the pressure of outlet port of rock core holder, its unit is MPa;

μ _g---high sulfur-containing natural gas viscosity under formation condition, its unit is mPas.

2, the liquid phase effective permeability K in each moment _scomputing formula be:

In formula, K _s---liquid phase effective permeability, its unit is mD;

μ _s---molten sulfur viscosity under formation condition, its unit is mPas;

Q _s---the molten sulfur flow at reservoir pressure, temperature, its unit is cm ³/ s.

3, the gas phase relative permeability K in each moment _rgcomputing formula be:

$K_{\mathrm{rg}}=\frac{K_g}{K_S\left(S_{\mathrm{wi}}\right)}$

In formula, K _rg---gas phase relative permeability;

S _wi---rock core sample irreducible water saturation.

4, the molten sulfur phase relative permeability K in each moment _rScomputing formula be:

$K_{\mathrm{rS}}=\frac{K_S}{K_S\left(S_{\mathrm{wi}}\right)}.$

5, the rock core sample exit end face in each moment is containing molten sulfur saturation degree S _scomputing formula be:

$S_S=\frac{{V^{\&prime;}}_{\mathrm{Si}}-V_{S0}}{V_P}$

In formula, V _s0---the volume of original measurement container molten sulfur, its unit is cm ³;

V _p---rock core sample volume of voids, its unit is cm ³.

6, the rock core sample exit end face gas saturation S in each moment _gcomputing formula be:

S _g＝1-S _wi-S _S。

Solution-air sulphur in described sub-step 2 oozes in test experiments mutually, when each injection is to the high sulfur-containing natural gas of certainty ratio and molten sulfur, the injection rate IR of often kind of fluid is at least 3 times of rock core sample volume of voids, and after the pressure at two ends of core holding unit is stable, then record experimental data.

Parameter high sulfur-containing natural gas formation condition Z-factor Z described in step 9 passes through Dranchuk-Abu-Kassem

(DAK) experimental formula computing method obtains, and its computing formula is:

$\begin{array}{c}1+(A_1+\frac{A_2}{T_{\mathrm{pr}}}+\frac{A_3}{T_{\mathrm{pr}}^3}+\frac{A_4}{T_{\mathrm{pr}}^4}+\frac{A_5}{T_{\mathrm{pr}}^5}){\mathrm{\&rho;}}_r+(A_6+\frac{A_7}{T_{\mathrm{pr}}}+\frac{A_8}{T_{\mathrm{pr}}^2}){\mathrm{\&rho;}}_r^2-\\ A_9(\frac{A_7}{T_{\mathrm{pr}}}+\frac{A_8}{T_{\mathrm{pr}}^2}){\mathrm{\&rho;}}_r^5+\frac{A_{10}}{T_{\mathrm{pr}}^3}{\mathrm{\&rho;}}_r^2(1+A_{11}{\mathrm{\&rho;}}_r^2)\exp (-A_{11}{\mathrm{\&rho;}}_r^2)-0.27\frac{p_{\mathrm{pr}}}{{\mathrm{\&rho;}}_r{T}_{\mathrm{pr}}}=0\end{array}$

$\begin{array}{c}Z=1+(A_1+\frac{A_2}{T_{\mathrm{pr}}}+\frac{A_3}{T_{\mathrm{pr}}^3}){\mathrm{\&rho;}}_r+(A_4+\frac{A_5}{T_{\mathrm{pr}}}){\mathrm{\&rho;}}_r^2+\left(\frac{A_5{A}_6}{T_{\mathrm{pr}}}\right){\mathrm{\&rho;}}_r^5\\ +\frac{A_7}{T_{\mathrm{pr}}^3}{\mathrm{\&rho;}}_r^2(1+A_8{\mathrm{\&rho;}}_r^2)\exp \left({-A}_8{\mathrm{\&rho;}}_r^2\right)\end{array}$

In formula, coefficient A ₁~ A ₁₁value be: A ₁=0.3265, A ₂=-1.07, A ₃=-0.5339, A ₄=0.01569, A ₅=-0.05165, A ₆=0.5475, A ₇=-0.7361, A ₈=0.1844, A ₉=0.1056, A ₁₀=0.6134, A ₁₁=0.721.

Work as T _prspan be 1.0≤T _prwhen≤3, p _prspan be 0.2≤p _pr≤ 30.

Work as T _prspan be 0.7≤T _prwhen≤1.0, p _prspan be p _pr<1.0.

Molten sulfur viscosity, mu under formation condition described in step 10 _spropose liquid sulfur viscosity experimental formula by people such as Shuai to calculate, its computing formula is:

${\mathrm{\&mu;}}_S=\left\{\begin{array}{cc}0.45271-2.0357\&times;{10}^{-3}T+2.3208\&times;{10}^{-6}{T}^2,& 392.1K<T<433.2K\\ 392350-2660.9T+6.0061T^2-4.5115\&times;{10}^{-3}{T}^3,& 433.2K<T<463.2K\\ \frac{108.03}{{(1+e^{0.0816(T-476.08)})}^{0.512}}+0.9423,& Y>463.2K\end{array}\right.$

In formula, μ _s---liquid sulfur viscosity, its unit is mPas;

T---temperature, its unit is K.

High sulfur-containing natural gas viscosity, mu under formation condition described in step 10 _g, calculated by Dempsey empirical formula method, its computing formula is:

$\begin{array}{c}\ln \left(\frac{{\mathrm{\&mu;}}_g{T}_r}{{\mathrm{\&mu;}}_1}\right)=A_0+A_1{p}_r+A_2{p}_r^2+A_3{p}_r^3+T_r(A_4+A_5{p}_r+A_6{p}_r^2+A_7{p}_r^3)\\ +T_r^2(A_8+A_9{p}_r+A_{10}{p}_r^2+A_{11}{p}_r^3)+T_r^3(A_{12}+A_{13}p+A_{14}{p}_r^2+A_{15}{p}_r^3)\\ {\mathrm{\&mu;}}_1=(1.709\&times;{10}^{-5}-2.062\&times;{10}^{-6}{\mathrm{\&gamma;}}_g)(1.8T+32)+8.188\&times;{10}^{-3}\\ -6.15\&times;{10}^{-3}\lg \left({\mathrm{\&gamma;}}_g\right)\end{array}$

In formula, parameter A ₀~ A ₁₅value be: A ₀=-2.4621182, A ₁=2.97054714, A ₂=-0.286264054, A ₃=0.00805420522, A ₄=2.80860949, A ₅=-3.49803305, A ₆=0.36037302, A ₇=-0.0104432413, A ₈=-0.793385684, A ₉=1.39643306, A ₁₀=-0.149144925, A ₁₁=0.00441015512, A ₁₂=0.0839387178, A ₁₃=-0.186408846, A ₁₄=0.0203367881, A ₁₅=-0.000609579263;

μ ₁---to place an order component gas viscosity at 1 atmospheric pressure with to fixed temperature, its unit is mPas;

γ _g---the relative density of high sulfur-containing natural gas, if the density of relative atmospheric is 1.

Claims (10)

1. High Temperature High Pressure acid gas reservoir gas-liquid sulphur phase percolation curve proving installation, is characterized in that: it comprises displacement system, formation condition simulation system, back pressure system, data acquisition system (DAS) and data testing system;

Described displacement system comprises sulfur-containing gas sample pot (1), nitrogen pot (2), gas boosting pump (5), gas sample intermediate receptacle (8), the first constant speed and constant pressure pump (12), molten sulfur intermediate receptacle (14), water sample intermediate receptacle (22), the second constant speed and constant pressure pump (19) and filtrator (16);

Described formation condition simulation system comprises core holding unit (27), automatically confined pressure and follows the trail of pump (46) and constant temperature oven (25);

Described back pressure system comprises back pressure control valve (30) and backpressure pump (31);

Described data testing system comprises high precision magnetic levitation balance (32), high temperature high voltage resistant gas-liquid separator (42), conical flask (44), condensation bath (34), gas meter (35) and tail gas neutralization pond (36);

Described data acquisition system (DAS) comprises multiple pressure transducer, temperature sensor (13), Thermostat Temperature Control instrument (24), gas meter (35), magnetic suspension balance sensor (47), data acquisition board (50) and computing machine (51);

The endpiece of the first constant speed and constant pressure pump (12) is connected with the inlet end of gas sample intermediate receptacle (8), the endpiece of gas sample intermediate receptacle (8) is connected with the endpiece of gas boosting pump (5) and the inlet end of core holding unit (27) respectively, and the endpiece of gas boosting pump (5) is connected with the endpiece of sulfur-containing gas sample pot (1) and nitrogen pot (2) respectively;

The endpiece of the second constant speed and constant pressure pump (19) is connected with the inlet end of water sample intermediate receptacle (22) and molten sulfur intermediate receptacle (14) respectively, the endpiece of water sample intermediate receptacle (22) is connected with the inlet end of core holding unit (27), and the endpiece of molten sulfur intermediate receptacle (14) is connected with the inlet end of core holding unit (27) by filtrator (16);

The endpiece of core holding unit (27) is connected with the inlet end of high temperature high voltage resistant gas-liquid separator (42) and back pressure control valve (30) respectively, the endpiece of back pressure control valve (30) is connected with the inlet end of backpressure pump (31), the endpiece that automatic confined pressure follows the trail of pump (46) is connected with the confined pressure input end of core holding unit (27), the liquid outlet end of high temperature high voltage resistant gas-liquid separator (42) is connected with the inlet end of conical flask (44), conical flask (44) hangs on high precision magnetic levitation balance (32), the gas outlet end of high temperature high voltage resistant gas-liquid separator (42) bathes (34) inlet end with condensation is connected, the endpiece of condensation bath (34) is connected with the inlet end of tail gas neutralization pond (36) by gas meter (35),

First constant speed and constant pressure pump (12) is provided with pressure transducer A (10), second constant speed and constant pressure pump (19) is provided with pressure transducer B (18), backpressure pump (31) is provided with pressure transducer C (29), the two ends of core holding unit (27) are respectively arranged with pressure transducer D (38) and pressure transducer E (40), automatic confined pressure is followed the trail of on pump (46) and is provided with pressure transducer F (45), molten sulfur intermediate receptacle (14) is provided with temperature sensor (13), constant temperature oven (25) is provided with Thermostat Temperature Control instrument (24), high precision magnetic levitation balance (32) is provided with magnetic suspension balance sensor (47), pressure transducer A (10), pressure transducer B (18), pressure transducer C (29), pressure transducer D (38), pressure transducer E (40), pressure transducer F (45), temperature sensor (13), Thermostat Temperature Control instrument (24), gas meter (35) is connected with the data input pin of data acquisition board (50) respectively with the data output end of magnetic suspension balance sensor (47), data acquisition board (50) is also connected with computing machine (51) and intercoms mutually,

Molten sulfur intermediate receptacle (14), water sample intermediate receptacle (22), gas sample intermediate receptacle (8), filtrator (16), core holding unit (27), conical flask (44) and high temperature high voltage resistant gas-liquid separator (42) are all arranged in constant temperature oven (25).

2. High Temperature High Pressure acid gas reservoir gas-liquid sulphur phase percolation curve proving installation according to claim 1, it is characterized in that: described gas sample intermediate receptacle (8) is also provided with emptying endpiece, and its emptying endpiece is connected with atmospheric valve (7).

3. High Temperature High Pressure acid gas reservoir gas-liquid sulphur phase percolation curve proving installation according to claim 1, it is characterized in that: described in be gas sample intermediate receptacle (8), water sample intermediate receptacle (22) and molten sulfur intermediate receptacle (14) be piston container, the interior separation of piston container is two not connected cavitys, upper end cavity is connected with the endpiece of piston container, and lower end cavity is connected with the inlet end of piston container.

4. High Temperature High Pressure acid gas reservoir gas-liquid sulphur phase percolation curve proving installation according to claim 3, it is characterized in that: described molten sulfur intermediate receptacle (14) is the device for solid-state sulphur being molten into molten sulfur, its arranged outside has ground heated filament heating arrangement, temperature sensor (13) on this ground heated filament heating arrangement.

5. High Temperature High Pressure acid gas reservoir gas-liquid sulphur phase percolation curve proving installation according to claim 1, it is characterized in that: the outside of described constant temperature oven (25) and condensation bath (34) and tail gas neutralization pond (36) is equipped with isolation tempered glass cover, and the upper end of this isolation tempered glass cover is also provided with hydrogen sulfide gas leakage warning device and explosion-proof exhaust fan.

6. High Temperature High Pressure acid gas reservoir gas-liquid sulphur phase percolation curve proving installation according to claim 1, is characterized in that: the two ends of described core holding unit (27) are parallel with differential pressure indicator (28).

7. High Temperature High Pressure acid gas reservoir gas-liquid sulphur phase percolation curve method of testing, is characterized in that: it comprises following multiple step:

Step 1, rock core is chosen and process: choose representational rock core sample, according to corresponding standard, rock core sample is carried out extracting, cleaning, drying and processing, measures the length L of described rock core sample, diameter d, core porosity φ, permeability K after process;

Step 2, the saturated local water of rock core: according to rock core sample actual formation water data preparation simulated formation aqueous solution, at normal temperatures the local water prepared is filled water sample intermediate receptacle (22), utilize experimental provision to vacuumize process to rock core sample;

Open the liquid control valve of the operation valve of the second constant speed and constant pressure pump (19), the inlet end operation valve of water sample intermediate receptacle (22), the endpiece operation valve of water sample intermediate receptacle (22), the inlet end operation valve of core holding unit (27), the endpiece operation valve of core holding unit (27) and high temperature high voltage resistant gas-liquid separator (42);

Close the gas control valve of the inlet end operation valve of molten sulfur intermediate receptacle (14), the operation valve of filtrator (16), the operation valve of gas sample intermediate receptacle (8), back pressure control valve (30), high temperature high voltage resistant gas-liquid separator (42);

Connect filling the water sample intermediate receptacle (22) of local water, core holding unit (27) and high temperature high voltage resistant gas-liquid separator (42), open the piston in the second constant speed and constant pressure pump (19) promotion water sample intermediate receptacle (22), by abundant for rock core sample saturated local water;

Step 3, Reality simulation stratum irreducible water condition: open the operation valve of nitrogen pot (2) and the operation valve of gas supercharge pump (5), by gas boosting pump (5), nitrogen is filled gas sample intermediate receptacle (8) at normal temperatures, then, the operation valve of nitrogen pot (2) and the operation valve of gas supercharge pump (5) is closed;

Close the endpiece operation valve of water sample intermediate receptacle (22), the operation valve of filtrator (16) and back pressure control valve (30);

Open the gas control valve of the operation valve of the first constant speed and constant pressure pump (12), the operation valve of gas sample intermediate receptacle (8), the inlet end operation valve of core holding unit (27), the endpiece operation valve of core holding unit (27), the liquid control valve of high temperature high voltage resistant gas-liquid separator (42) and high temperature high voltage resistant gas-liquid separator (42);

Connect gas sample intermediate receptacle (8), core holding unit (27) and the high temperature high voltage resistant gas-liquid separator (42) of filling nitrogen, first follow the trail of pump (46) by automatic confined pressure before displacement running and load certain confined pressure to core holding unit (27), open the piston in the first constant speed and constant pressure pump (12) promotion gas sample intermediate receptacle (8), nitrogen flooding is made to replace local water in rock core sample, displace local water, until the liquid outlet end of high temperature high voltage resistant gas-liquid separator (42) does not go out local water, displacement process terminates;

Step 4, molten sulfur prepares: the high sulfur-containing natural gas sample choosing actual acid gas reservoir, the atmospheric valve of gas sample intermediate receptacle (7) is first opened before injecting sample gas, the remaining nitrogen of dropping a hint in sample intermediate receptacle (7), then close the atmospheric valve of sample intermediate receptacle (7) of holding one's breath, under normal temperature, by gas boosting pump (5), gas sample intermediate receptacle (8) is filled the high pressure sulfur-containing gas of reservoir pressure; According to actual gas reservoir sulfur component, choose corresponding solid-state sulphur, and put it into the molten sulfur intermediate receptacle (14) of high temperature, by the mode of molten sulfur intermediate receptacle (14) conducting self-heating, make solid-state sulphur reach fusing point fusing and form liquid sulfur;

Step 5, simulated formation high temperature and high pressure environment: follow the trail of pump (46) by automatic confined pressure and load the simulation stratum condition confined pressure set to core holding unit (27); Utilize constant temperature oven (25) simulated formation high temperature, and ensure to there will not be in whole molten sulfur displacement process solidification and blocking pipeline and rock core sample;

Step 6, determine the condition of the molten sulfur phase permeability under irreducible water saturation:

Open the gas control valve of the operation valve of the second constant speed and constant pressure pump (19), the inlet end operation valve of molten sulfur intermediate receptacle (14), the endpiece operation valve of molten sulfur intermediate receptacle (14), the operation valve of filtrator (16), the inlet end operation valve of core holding unit (27), the endpiece operation valve of core holding unit (27), the liquid control valve of high temperature high voltage resistant gas-liquid separator (42) and high temperature high voltage resistant gas-liquid separator (42);

Close the inlet end operation valve of water sample intermediate receptacle (19), the endpiece operation valve of water sample intermediate receptacle (19), the operation valve of gas sample intermediate receptacle (8) and back pressure control valve (30);

Connect molten sulfur intermediate receptacle (14), core holding unit (27) and high temperature high voltage resistant gas-liquid separator (42) that high temperature molten sulfur is housed; Open the piston in the second constant speed and constant pressure pump (19) promotion molten sulfur intermediate receptacle (14), the rock core sample of the molten sulfur displacement irreducible water in molten sulfur intermediate receptacle (14);

Step 7: adopt the second constant speed and constant pressure pump (19) to carry out the displacement of constant voltage molten sulfur, after the volume of voids that constant voltage displacement reaches 10 times, the pressure reduction imported and exported until core holding unit (27) two ends and rate of discharge stable after, timing determines oral fluid sulphur flow, METHOD FOR CONTINUOUS DETERMINATION three molten sulfur phase permeabilities, its relative error is less than 3%, with this molten sulfur phase permeability K _s, as solution-air sulphur relative permeability basis; The computing formula of the molten sulfur phase permeability under irreducible water saturation is:

In formula: K _s---molten sulfur phase effective permeability under irreducible water state, its unit is mD;

B _s---the molten sulfur volume factor under formation temperature, pressure condition;

Q _s---the flow of molten sulfur under rock core top hole pressure, its unit is mL/s;

μ _s---the viscosity of molten sulfur under formation temperature, pressure condition, its unit is mPas;

L---rock core sample length, its unit is cm;

A---rock core sample sectional area, its unit is cm ²;

P ₁---rock core sample intake pressure, its unit is MPa;

P ₂---rock core sample top hole pressure, its unit is MPa;

S _wi---rock core sample irreducible water saturation;

Step 8, what solution-air sulphur injected in setting ratio oozes test mutually, and it comprises following multiple sub-step:

Sub-step 1: the operation valve opening the first constant speed and constant pressure pump (12), the operation valve of the second constant speed and constant pressure pump (19), the inlet end operation valve of molten sulfur intermediate receptacle (14), the endpiece operation valve of molten sulfur intermediate receptacle (14), the operation valve of filtrator (16), the operation valve of gas sample intermediate receptacle (8), the inlet end operation valve of core holding unit (27), the endpiece operation valve of core holding unit (27), the liquid control valve of high temperature high voltage resistant gas-liquid separator (42), the gas control valve of high temperature high voltage resistant gas-liquid separator (42) and back pressure control valve (30),

Close operation valve, the inlet end operation valve of water sample intermediate receptacle (22), the endpiece operation valve of water sample intermediate receptacle (22) of gas boosting pump (5), connect gas sample intermediate receptacle (8), molten sulfur intermediate receptacle (14), core holding unit (27) and the high temperature high voltage resistant gas-liquid separator (42) of filling high sulfur-containing natural gas;

Sub-step 2: simultaneously start the first constant speed and constant pressure pump (12) and the second constant speed and constant pressure pump (19), set constant speed or constant voltage, the endpiece of core holding unit (27) sets back pressure, high sulfur-containing natural gas and molten sulfur are injected core holding unit (27) with the ratio set, start solution-air sulphur and ooze test experiments mutually, the endpiece of core holding unit (27) is by high temperature high voltage resistant gas-liquid separator (42), molten sulfur and gas are carried out gas-liquid separation, the endpiece of high temperature high voltage resistant gas-liquid separator gas (42) is through condensation bath (34), water vapour is mixed with in removing gas, the gas flow of condensation bath (34) endpiece is measured by gas meter (35), molten sulfur flows into conical flask (44) from the liquid outlet end of high temperature high voltage resistant gas-liquid separator (42), under this conical flask (44) hangs on high precision magnetic levitation balance (32), be in suspended state, measure not molten sulfur quality in the same time by high precision magnetic levitation balance (32), calculate corresponding molten sulfur amount,

Sub-step 3: after experiment is less than 0.005 to high sulfur-containing natural gas phase effective permeability permeability, measures molten sulfur phase effective permeability and terminates experiment;

Step 9, record accumulation production fluid sulfur content V _siwith tolerance V _giand carry out formation condition correction: the inlet and outlet pressure P recording the different injection ratio rock core two ends of two kinds of fluids ₁, P ₂accumulation production fluid sulfur content V under the top hole pressure condition of differential pressure Δ P and rock clamper (27) _siwith tolerance V _gi;

By the volume factor of corresponding formation condition fluid surface condition semi-invariant changed into the amount under formation condition, its computing formula related to is:

V' _Si＝V _SiB _S

V' _gi＝(V _gi-V _SiR _SG)B _G

In formula: V' _si---accumulation production fluid sulfur content under two kinds of fluid a certain injection ratio formation conditions after correction, its unit is cm ³;

V' _gi---cumulative gas production under two kinds of fluid a certain injection ratio formation conditions after correction, its unit is cm ³;

V _si---accumulation production fluid sulfur content under two kinds of fluid a certain injection ratio formation conditions, its unit is cm ³;

V _gi---cumulative gas production under two kinds of fluid a certain injection ratio formation conditions, its unit is cm ³;

R _sG---the original solution gas liquor ratio of molten sulfur;

B _s---molten sulfur initial volume coefficient;

B _g---high sulfur-containing natural gas initial volume coefficient;

Wherein, the original solution gas liquor ratio R of molten sulfur _sGwith molten sulfur initial volume coefficient B _smeasured by PVT tester, its computing formula is:

In formula: W _s---the quality of degassed molten sulfur, its unit is g;

ρ _s---the density of degassed molten sulfur under surface temperature, its unit is g/cm ³;

V _g---the volume in molten sulfur under the isolated status of criterion, its unit is cm ³;

V _s---release the subsurface volume of molten sulfur, its unit is cm ³;

Wherein, high sulfur-containing natural gas initial volume coefficient B _gcomputing formula be:

In formula: Z---high sulfur-containing natural gas formation condition Z-factor;

T---formation temperature, its unit is DEG C;

P---reservoir pressure, its unit is MPa;

P _sC---surface air pressure, its unit is MPa;

Step 10, calculates the molten sulfur phase relative permeability K in each moment _rs, gas phase relative permeability K _rgwith core sample gas saturation S _g:

1. the gas phase effective permeability K in each moment _gcomputing formula be:

In formula, K _g---gas phase effective permeability, its unit is mD;

A---the sectional area of rock core sample, its unit is cm ²;

P _a---atmospheric pressure, its unit is MPa;

L---the length of rock core sample, its unit is cm;

Q _g---the high sulfur-containing natural gas flow at reservoir pressure, temperature, its unit is cm ³/ s;

P ₁---the pressure of core holding unit inlet end, its unit is MPa;

P ₂---the pressure of outlet port of rock core holder, its unit is MPa;

μ _g---high sulfur-containing natural gas viscosity under formation condition, its unit is mPas;

2. the liquid phase effective permeability K in each moment _scomputing formula be:

In formula, K _s---liquid phase effective permeability, its unit is mD;

μ _s---molten sulfur viscosity under formation condition, its unit is mPas;

Q _s---the molten sulfur flow at reservoir pressure, temperature, its unit is cm ³/ s;

3. the gas phase relative permeability K in each moment _rgcomputing formula be:

In formula, K _rg---gas phase relative permeability;

S _wi---rock core sample irreducible water saturation;

4. the molten sulfur phase relative permeability K in each moment _rScomputing formula be:

5. the rock core sample exit end face in each moment is containing molten sulfur saturation degree S _scomputing formula be:

In formula, V _s0---the volume of original measurement container molten sulfur, its unit is cm ³;

V _p---rock core sample volume of voids, its unit is cm ³;

6. the rock core sample exit end face gas saturation S in each moment _gcomputing formula be:

S _g＝1-S _wi-S _S。

8. High Temperature High Pressure acid gas reservoir gas-liquid sulphur phase percolation curve method of testing according to claim 7, it is characterized in that: the solution-air sulphur in described sub-step 2 oozes in test experiments mutually, when each injection is to the high sulfur-containing natural gas of certainty ratio and molten sulfur, the injection rate IR of often kind of fluid is at least 3 times of rock core sample volume of voids, and after the pressure at two ends of core holding unit (27) is stable, then record experimental data.

9. High Temperature High Pressure acid gas reservoir gas-liquid sulphur phase percolation curve method of testing according to claim 7, it is characterized in that: the parameter high sulfur-containing natural gas formation condition Z-factor Z described in step 9 is obtained by Dranchuk-Abu-Kassem experimental formula computing method, and its computing formula is:

In formula, coefficient A ₁~ A ₁₁value be: A ₁=0.3265, A ₂=-1.07, A ₃=-0.5339, A ₄=0.01569, A ₅=-0.05165, A ₆=0.5475, A ₇=-0.7361, A ₈=0.1844, A ₉=0.1056, A ₁₀=0.6134, A ₁₁=0.721;

Work as T _prspan be 1.0≤T _prwhen≤3, p _prspan be 0.2≤p _pr≤ 30;

Work as T _prspan be 0.7≤T _prwhen≤1.0, p _prspan be p _pr<1.0.

10. High Temperature High Pressure acid gas reservoir gas-liquid sulphur phase percolation curve method of testing according to claim 7, is characterized in that:

Molten sulfur viscosity, mu under formation condition described in step 10 _scalculated by liquid sulfur viscosity experimental formula, its computing formula is:

In formula, μ _s---liquid sulfur viscosity, its unit is mPas;

T---temperature, its unit is K;

High sulfur-containing natural gas viscosity, mu under formation condition described in step 10 _g, calculated by Dempsey empirical formula method, its computing formula is:

In formula, parameter A ₀~ A ₁₅value be: A ₀=-2.4621182, A ₁=2.97054714, A ₂=-0.286264054, A ₃=0.00805420522, A ₄=2.80860949, A ₅=-3.49803305, A ₆=0.36037302, A ₇=-0.0104432413, A ₈=-0.793385684, A ₉=1.39643306, A ₁₀=-0.149144925, A ₁₁=0.00441015512, A ₁₂=0.0839387178, A ₁₃=-0.186408846, A ₁₄=0.0203367881, A ₁₅=-0.000609579263;

μ ₁---to place an order component gas viscosity at 1 atmospheric pressure with to fixed temperature, its unit is mPas;

γ _g---the relative density of high sulfur-containing natural gas.