WO2019007163A1 - 一种含硫气体中的元素硫溶解度的测定装置及方法 - Google Patents
一种含硫气体中的元素硫溶解度的测定装置及方法 Download PDFInfo
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- WO2019007163A1 WO2019007163A1 PCT/CN2018/088415 CN2018088415W WO2019007163A1 WO 2019007163 A1 WO2019007163 A1 WO 2019007163A1 CN 2018088415 W CN2018088415 W CN 2018088415W WO 2019007163 A1 WO2019007163 A1 WO 2019007163A1
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- Prior art keywords
- sulfur
- containing gas
- tank
- sampling
- pressure
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- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 title claims abstract description 275
- 238000000034 method Methods 0.000 title claims abstract description 35
- 239000005864 Sulphur Substances 0.000 title abstract 4
- 238000001179 sorption measurement Methods 0.000 claims abstract description 88
- 238000004891 communication Methods 0.000 claims abstract description 54
- 238000006073 displacement reaction Methods 0.000 claims abstract description 21
- 229910052717 sulfur Inorganic materials 0.000 claims description 170
- 239000011593 sulfur Substances 0.000 claims description 170
- 238000005070 sampling Methods 0.000 claims description 121
- QGJOPFRUJISHPQ-UHFFFAOYSA-N Carbon disulfide Chemical compound S=C=S QGJOPFRUJISHPQ-UHFFFAOYSA-N 0.000 claims description 114
- 239000007788 liquid Substances 0.000 claims description 42
- 238000002347 injection Methods 0.000 claims description 11
- 239000007924 injection Substances 0.000 claims description 11
- 238000011084 recovery Methods 0.000 claims description 11
- 238000001802 infusion Methods 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 6
- QGJOPFRUJISHPQ-NJFSPNSNSA-N carbon disulfide-14c Chemical compound S=[14C]=S QGJOPFRUJISHPQ-NJFSPNSNSA-N 0.000 claims description 5
- 238000005303 weighing Methods 0.000 claims description 3
- 239000007789 gas Substances 0.000 description 217
- 238000002474 experimental method Methods 0.000 description 5
- 238000010521 absorption reaction Methods 0.000 description 4
- 150000003463 sulfur Chemical class 0.000 description 4
- 239000012530 fluid Substances 0.000 description 3
- 239000011261 inert gas Substances 0.000 description 3
- 238000012546 transfer Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 108010010803 Gelatin Proteins 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 239000010426 asphalt Substances 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 229920000159 gelatin Polymers 0.000 description 2
- 239000008273 gelatin Substances 0.000 description 2
- 235000019322 gelatine Nutrition 0.000 description 2
- 235000011852 gelatine desserts Nutrition 0.000 description 2
- 230000008676 import Effects 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 238000011109 contamination Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- -1 nitrogen Chemical compound 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Images
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/0004—Gaseous mixtures, e.g. polluted air
- G01N33/0009—General constructional details of gas analysers, e.g. portable test equipment
- G01N33/0027—General constructional details of gas analysers, e.g. portable test equipment concerning the detector
- G01N33/0036—General constructional details of gas analysers, e.g. portable test equipment concerning the detector specially adapted to detect a particular component
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N7/00—Analysing materials by measuring the pressure or volume of a gas or vapour
- G01N7/02—Analysing materials by measuring the pressure or volume of a gas or vapour by absorption, adsorption, or combustion of components and measurement of the change in pressure or volume of the remainder
- G01N7/04—Analysing materials by measuring the pressure or volume of a gas or vapour by absorption, adsorption, or combustion of components and measurement of the change in pressure or volume of the remainder by absorption or adsorption alone
Definitions
- the invention relates to a device and a method for measuring the solubility of elemental sulfur in a sulfur-containing gas, and belongs to the technical field of oil and gas exploitation.
- an object of the present invention is to provide an apparatus for measuring the solubility of elemental sulfur in a sulfur-containing gas.
- the present invention provides a device for measuring the solubility of elemental sulfur in a sulfur-containing gas, the device comprising a displacement pump, a first sampler, a high temperature tank, a back pressure pump, a control valve, a adsorption tank, a cryostat, a flow meter, and a collection canister, wherein an outlet of the displacement pump is in communication with an inlet of the first sampler, and an outlet of the first sampler is in communication with a first inlet of the control valve, a second inlet of the control valve is in communication with an outlet of the back pressure pump, an outlet of the control valve is in communication with a first opening of the canister, and a second opening of the canister is in communication with the flow meter; a third opening of the canister is in communication with the collection canister;
- the first sampler is located in the high temperature tank, the adsorption tank is located in the low temperature tank, a valve is disposed between an outlet of the first sampler and a first inlet of the control valve, and the adsorption A valve is disposed between the third opening of the canister and the collection canister, the collection canister being adapted to be heated.
- the apparatus further includes a sampler, an outlet of the first sampler is in communication with an inlet of the sampler, an outlet of the sampler and the control valve The first inlet is in communication and the sampler is located in the high temperature tank.
- the apparatus further, if the sampler contains sulfur powder, the apparatus further includes a rocking device connected to the sampler.
- the rocking device is a conventional device used in the art and its connection with the sampler is also a conventional connection in the art, and the device provided by the present application is installed with the purpose of keeping the sampler at a constant temperature. Swing under constant pressure.
- a filter is arranged between the outlet of the sampler and the first inlet of the control valve.
- the apparatus further includes a second sampler, an inlet of the second sampler being in communication with the displacement pump, an outlet of the second sampler and the control valve The first import is connected.
- a filter is disposed between the second sampler and the first inlet of the control valve.
- a first coil is disposed between the outlet of the control valve and the first opening of the canister, and the first coil is located in the cryostat.
- a second coil is disposed between the second opening of the canister and the flow meter.
- the flow meter is at least two, and the at least two flow meters are connected in parallel after the second coil, each flow meter and the second coil There are pneumatic valves connected between them.
- the outlet of the flow meter is in communication with the exhaust gas treatment tank.
- the apparatus further includes a liquefaction tank, the liquefaction tank being located in the low temperature tank, the collection tank being in communication with an inlet of the liquefaction tank, the collection tank and the A check valve is provided on the line between the liquefaction tanks to flow from the collection tank to the liquefaction tank.
- the apparatus further includes a recovery tank and an infusion pump, the recovery tank and the infusion pump being in communication with an outlet of the liquefaction tank, respectively.
- the infusion pump is in communication with the third opening of the canister.
- the infusion pump is connected between the sampler and the first inlet of the control valve.
- the present invention also provides a method for determining the solubility of elemental sulfur in a sulfur-containing gas to obtain the elemental sulfur solubility in a sulfur-containing gas relatively accurately.
- the gas flowing out of the adsorption tank passes through a gas flow meter that determines a volume of the sulfur-containing gas at room temperature and the chamber pressure;
- outlet of the sampler is in communication with the inlet of the back pressure valve
- the outlet of the back pressure valve is in communication with the inlet of the adsorption tank
- the first outlet of the adsorption tank is in communication with the flow meter
- the sampler is located in the high temperature tank, the adsorption tank is located in the low temperature tank, and a valve is disposed between an outlet of the sampler and an inlet of the back pressure valve, and the collection tank is suitable It is heated.
- the volume according to the sampling temperature, the sampling pressure, the room temperature, the chamber pressure, the mass of the elemental sulfur, and the volume of the sulfur-containing gas at the room temperature and the chamber pressure Calculating the solubility of elemental sulfur in the sulfur-containing gas, including:
- the solubility of the elemental sulfur in the sulfur-containing gas is calculated based on the volume of the sulfur-containing gas at the sampling temperature and the sampling pressure and the mass of the elemental sulfur.
- the volume of the sulfur-containing gas in a standard state is calculated according to the room temperature, the chamber pressure, and a volume of the sulfur-containing gas at the room temperature and the chamber pressure. Calculated as follows:
- V 0 the volume of the sulfur-containing gas in the state of the standard
- V 1 the volume of sulfur-containing gas at room temperature and chamber pressure
- the volume of the sulfur-containing gas at the sampling temperature and the sampling pressure is calculated according to a volume of the sulfur-containing gas in a state, a sampling temperature, and the sampling pressure, and
- the calculation formula is:
- V' 1 the volume of the sulfur-containing gas at the sampling temperature and the sampling pressure
- V 0 the volume of the sulfur-containing gas in the state of the standard
- T sampling temperature
- the solubility of the elemental sulfur in the sulfur-containing gas is calculated according to the volume of the sulfur-containing gas at the sampling temperature and the sampling pressure and the mass of the elemental sulfur, and the calculation formula is:
- V' 1 the volume of the sulfur-containing gas at the sampling temperature and sampling pressure.
- the method further comprises:
- a line between the sampler and the adsorption tank is washed with a carbon disulfide liquid, and the washed carbon disulfide liquid is collected and transferred into the collection tank.
- an outlet of the gas flow meter is connected to an exhaust gas absorption tank.
- the lower end of the adsorption tank is provided with a second outlet, the second outlet of the adsorption tank is connected to the collection tank through a pipeline, and the pipeline between the adsorption tank and the collection tank is arranged There are valves.
- the present invention also provides a method for determining the solubility of elemental sulfur in a sulfur-containing gas, comprising:
- step (2) (2) reducing the sulfur-containing gas in step (1) to a chamber pressure, and then adsorbing the sulfur-containing gas using a carbon disulfide liquid;
- step (2) measuring step (2) the volume of the sulfur-containing gas obtained after adsorption at room temperature and the pressure of the chamber;
- the step (5) is performed according to the sampling temperature, the sampling pressure, the room temperature, the chamber pressure, the mass of the elemental sulfur, and the step (2) after adsorption.
- the solubility of the elemental sulfur in the sulfur-containing gas is calculated based on the volume of the sulfur-containing gas at the sampling temperature and the sampling pressure and the mass of the elemental sulfur.
- the volume is calculated according to the room temperature, the chamber pressure, and the volume of the sulfur-containing gas obtained after the adsorption in the step (2) at the room temperature and the chamber pressure.
- the volume of the sulfur-containing gas in the standard state includes calculating the volume of the sulfur-containing gas in the standard state by using the following formula (1);
- V 0 the volume of the sulfur-containing gas in the state of the standard
- V 1 the volume of sulfur-containing gas at room temperature and chamber pressure
- the sulfur-containing gas is calculated at the sampling temperature and
- the volume under the sampling pressure includes calculating the volume of the sulfur-containing gas at the sampling temperature and the sampling pressure by using the following formula (2);
- V' 1 the volume of the sulfur-containing gas at the sampling temperature and the sampling pressure
- V 0 the volume of the sulfur-containing gas in the state of the standard
- T sampling temperature
- the element in the sulfur-containing gas is calculated according to the volume of the sulfur-containing gas at the sampling temperature and the sampling pressure and the mass of the elemental sulfur.
- the solubility of sulfur includes the solubility of elemental sulfur in the sulfur-containing gas calculated by the following formula (3);
- V' 1 the volume of the sulfur-containing gas at the sampling temperature and sampling pressure.
- the method specifically comprises the following steps:
- step (3) reducing the sulfur-containing gas in step (2) to a chamber pressure, and then flowing into the adsorption tank, wherein the adsorption tank contains a carbon disulfide liquid;
- the gas flowing out of the adsorption tank passes through a gas flow meter, and the gas flow meter measures the volume of the sulfur-containing gas obtained in the step (3) at room temperature and the chamber pressure;
- the method further comprises:
- the pipeline between the sampler and the adsorption tank is washed with a carbon disulfide liquid, and the washed carbon disulfide liquid is collected and transferred into the collection tank.
- the method and device for measuring the solubility of elemental sulfur in the sulfur-containing gas can drive the sulfur-containing gas in the first sampler to the control valve through the displacement pump, and adjust the pressure of the back pressure pump to make the gas pass through
- the control valve realizes balanced depressurization and smooth outflow, thereby ensuring accurate gas flow measured by the flowmeter;
- the first sampler is located in the high temperature tank, which can prevent elemental sulfur in the gas from being precipitated, and the measurement result is accurate;
- the adsorption tank is located at a low temperature. In the tank, it is ensured that the elemental sulfur in the gas is sufficiently adsorbed in the adsorption tank; the content of elemental sulfur in the gas can be obtained by heating the collection tank.
- the content of elemental sulfur in the gas measured by the device and the method provided by the invention is relatively accurate, and the elemental sulfur in the sulfur-containing gas is calculated based on the gas flow rate measured by the device and the method and the elemental sulfur content in the gas.
- the solubility is relatively accurate.
- FIG. 1 is a schematic structural view of an apparatus for measuring the solubility of elemental sulfur in a sulfur-containing gas according to an embodiment of the present invention
- FIG. 2 is a schematic structural view of an apparatus for measuring the solubility of elemental sulfur in a sulfur-containing gas according to another embodiment of the present invention
- FIG. 3 is a process flow diagram of a method for determining the solubility of elemental sulfur in a sulfur-containing gas according to an embodiment of the present invention.
- the embodiment provides a measuring device for the solubility of elemental sulfur in a sulfur-containing gas, which comprises a displacement pump 1, a first sampler 6, a high temperature tank 18, a back pressure pump 21, a control valve 20, a adsorption tank 23, and a low temperature. a tank 48, a flow meter, and a collection tank 35, wherein
- the outlet of the displacement pump 1 is in communication with the inlet of the first sampler 6, the outlet of the first sampler 6 is in communication with the first inlet of the control valve 20, and the second inlet of the control valve 20 is in communication with the outlet of the return pump 21, controlled
- the outlet of the valve 20 is in communication with the first opening of the canister 23, the second opening of the canister 23 is in communication with the flow meter; the third opening of the canister 23 is in communication with the collection canister 35;
- the first sampler 6 is located in the high temperature tank 18, the adsorption tank 23 is located in the low temperature tank 48, the fifth valve 7 is disposed between the outlet of the first sampler 6 and the first inlet of the control valve 20, and the third of the adsorption tank 23 A fourteenth valve 32 is provided between the opening and the collection tank 35, and the collection tank 35 is adapted to be heated.
- the communication between adjacent devices can be realized by a pipeline, but the present invention is not limited thereto, and may be directly connected or otherwise realized.
- the description of one device in communication with another device means that the two can be connected by conduit, directly connected, or other suitable means.
- the gas to be tested is first placed in the first sampler 6, the sixth valve 9 is first closed, and the back pressure pump 21 is opened to make the water in the back pressure pump 21 from the control valve 20.
- the second inlet enters, then opens the sixth valve 9, the gas to be tested enters from the first inlet of the control valve 20, and then adjusts the pressure of the back pressure pump 21 so that the pressure of the gas passing through the control valve 20 and the pressure of the back pressure pump 21
- the pressure difference of the back pressure is in the range of 0.1 MPa, so that the gas is balanced and pressure-reduced through the control valve 20, and the gas smoothly flows out from the control valve 20 and enters the adsorption tank 23.
- the carbon disulfide liquid in the adsorption tank 23 adsorbs elemental sulfur in the sulfur-containing gas.
- the gas flowing out of the adsorption tank 23 enters the flow meter, and the flow meter can measure the volume of the gas.
- the fourteenth valve 32 between the adsorption tank 23 and the collection tank 35 is opened, and the carbon disulfide liquid in the adsorption tank 23 flows into the collection tank 35, and then the collection tank 35 is heated, and carbon disulfide becomes a gas volatilization, and elemental sulfur remains.
- the mass of the elemental sulfur can be obtained by weighing.
- the solubility of elemental sulfur in the high sulfur content gas can be calculated by combining the model.
- the first sampler 6 is located in the high temperature tank 18 to ensure that elemental sulfur in the gas does not precipitate; and the adsorption tank 23 is located in the low temperature tank 48, so that the carbon disulfide liquid in the adsorption tank 23 is not volatilized, and The elemental sulfur is sufficiently adsorbed in the adsorption tank 23, and therefore the apparatus provided by the present invention can relatively accurately measure the solubility of elemental sulfur in the gas.
- the high temperature tank 18 may be an air bath high temperature tank or other forms of high temperature tank.
- the present embodiment provides a device for measuring the solubility of elemental sulfur in a sulfur-containing gas.
- the structure of the device is shown in FIG. 2.
- the apparatus of the embodiment further includes a sampler 8 and a rocking device, the inlet of the first sampler 6 is in communication with the outlet of the displacement pump 1, and the outlet of the first sampler 6 is in communication with the inlet of the sampler 8, the sampler The outlet of 8 is in communication with the first inlet of the control valve 20, and the sampler 8 is located within the high temperature tank 18 and is coupled to the rocking device.
- a sixth valve 9 is disposed between the sampler 8 and the control valve 20, and a fifth valve 7 and a seventh valve 10 are disposed between the first sampler 6 and the sampler 8, and the first sampler 6 and the displacement
- a second valve 3 is provided between the pumps 1.
- the first sampler 6 can be placed outside the high temperature tank 18, and when it is necessary to measure the solubility of elemental sulfur in the gas in the first sampler 6, The gas in the first sampler 6 is displaced into the sampler 8 in the high temperature tank 18.
- the sixth valve 9 When it is necessary to determine the solubility of the elemental sulfur in the saturated sulfur-containing gas, the sixth valve 9 is closed, the second valve 3, the fifth valve 7 and the seventh valve 10 are opened, and the displacement pump 1 drives the gas in the first sampler 6 The second valve 3, the fifth valve 7, and the seventh valve 10 are then closed in the same. An excessive amount of sulfur powder is placed in the sampler 8, and the rocking device is turned on to sway the sampler 8 in a constant temperature and constant pressure state for 24 hours to ensure that elemental sulfur in the saturated sulfur-containing gas does not precipitate.
- a third valve 4 is disposed between the sampler 8 and the outlet of the displacement pump 1 to open the third valve 4, and the displacement pump 1 drives the saturated sulfur-containing gas in the sampler 8 from the first inlet of the control valve 20.
- the pressure of the back pressure pump 21 is adjusted, so that the saturated sulfur-containing gas is balanced and depressurized through the control valve 20 and smoothly flows into the adsorption tank.
- a branch is provided on the line between the displacement pump 1 and the sampler 8, and a fourth valve 5 is provided on the branch, and the fourth valve 5 is used to discharge water in the sampler 8.
- an emergency brake valve 19 may be disposed between the first inlet of the control valve 20 and the sampler 8 and the first sampler 6, that is, the emergency brake valve 19 can simultaneously stop the sampler 8 to The circulation of the first inlet of the control valve 20.
- the emergency brake valve 19 can be closed to avoid damage to the flow meter.
- a second filter 16 is disposed between the outlet of the sampler 8 and the first inlet of the control valve 20.
- the second filter 16 can filter out acid, asphalt, gelatin, and the like from the gas flowing out of the sampler 8 to avoid clogging of the pipeline.
- the second filter 16 and the third filter 17 can be connected in parallel to be connected between the sampler 8 and the control valve 20.
- a ninth valve 14 is disposed between the sampler 8 and the second filter 16, and a tenth valve 15 is disposed between the sampler 8 and the third filter 17. The ninth valve 14 and the tenth valve 15 are opened, and the gas in the sampler 8 passes through the second filter 16 and the third filter 17, respectively, and flows into the control valve 20.
- the apparatus further includes a second sampler 11, the inlet of the second sampler 11 is in communication with the displacement pump 1, the outlet of the second sampler 11 and the control valve 20 are An import is connected.
- the second sampler 11 can be a downhole sampler, and the gas sample taken out from the well is under a large pressure, and the balance is directly reduced by the control valve 20.
- a first filter 12 is disposed between the second sampler 11 and the first inlet of the control valve 20.
- the first filter 12 can filter out acid, asphalt, gelatin, and the like from the gas flowing out of the second sampler 11 to avoid clogging of the pipeline.
- a first valve 2 is disposed between the displacement pump 1 and the second sampler 11, and an eighth valve 13 is disposed between the second sampler 11 and the control valve 20.
- the first valve 2 and the eighth valve 13 are opened, and the displacement pump 1 drives the gas in the second sampler 11 to flow through the control valve 20.
- a first coil 22 is disposed between the outlet of the control valve 20 and the inlet of the canister 23, and the first coil 22 is located in the low temperature tank 48.
- the gas flowing out of the control valve 20 can be cooled first in the first coil 22 and then into the adsorption tank 23 to prevent the temperature of the gas entering the adsorption tank 23 from being too high to cause the carbon disulfide to volatilize.
- a second coil 36 is disposed between the second opening of the canister 23 and the flow meter.
- the gas flowing out of the adsorption tank 23 can first reduce the gas velocity through the second coil 36, and avoid the gas flow rate being too high to cause the flowmeter to over-range.
- the flowmeters are three, and after the three flowmeters are connected in parallel and connected to the second coil 36, a pneumatic valve is connected between each flowmeter and the second coil 36. .
- the first flow meter 38 is in series with the first pneumatic valve 37
- the second flow meter 40 is in series with the second pneumatic valve 39
- the third flow meter 42 is in series with the third pneumatic valve 41.
- the flowmeters of the three flowmeters are different, and the flowmeter of the appropriate range can be selected according to the needs, thereby ensuring that the measured gas flow rate is more accurate.
- Gas is introduced into the designated flow meter by controlling the first pneumatic valve 37, the second pneumatic valve 39, and the third pneumatic valve 41. This embodiment is described by the number of flow meters being three, but the present invention is not limited thereto.
- the outlet of the flow meter is in communication with the exhaust gas treatment tank 46.
- a fourth check valve 44 is disposed between the exhaust gas treatment tank 46 and the flow meter. When gas flows out from the outlet of the flow meter, the fourth check valve 44 is opened, so that the gas can enter the exhaust gas treatment tank 46 to prevent pollution. surroundings.
- a sixth check valve 47 is provided on the outlet line of the exhaust gas treatment tank 46. The sixth check valve 47 is opened, and the gas treated by the exhaust gas treatment tank 46 can flow into other devices.
- the apparatus further includes a liquefaction tank 25 located in the low temperature tank 48, the collection tank 35 is in communication with the inlet of the liquefaction tank 25, and between the collection tank 35 and the liquefaction tank 25.
- a third check valve 33 is provided on the line to flow from the collection tank 35 to the liquefaction tank 25.
- a fifteenth valve 34 is disposed on the pipeline communicating with the collection tank 35. When the collection tank 35 is heated, the fifteenth valve 34 is opened and an inert gas which is dry and does not react with elemental sulfur and carbon disulfide, such as nitrogen, is inert. The gas carries all of the carbon disulfide gas in the collection tank 35 from the collection tank 35 and enters the liquefaction tank 25.
- the carbon disulfide gas entering the liquefaction tank 25 is liquefied and deposited to the lower portion of the liquefaction tank 25.
- a sixteenth valve 43 is provided between the outlet of the upper end of the liquefaction tank 25 and the exhaust gas treatment tank 46, and the sixteenth valve 43 is opened, and the inert gas is discharged from the upper end of the liquefaction tank 25 and enters the exhaust gas treatment tank 46.
- the outlet of the upper end of the liquefaction tank 25 is connected to the fifth one-way valve 45 through a pipeline.
- a fourth one-way valve 44 is required between the fifth one-way valve 45 and the flow meter, and the sixteenth valve 43 is opened.
- the fourth check valve 44 needs to be closed to prevent inert gas from flowing back into the flow meter.
- the apparatus further includes a recovery tank 29 and an infusion pump 28, and the recovery tank 29 and the infusion pump 28 are in communication with the outlet of the liquefaction tank 25, respectively.
- a first check valve 27 is disposed in the line leading to the recovery tank 29 and the liquid injection pump 28 in the liquefaction tank 25, and the first check valve 27 is opened, and the carbon disulfide liquid in the liquefaction tank 25 flows to the liquid injection pump 28 and the recovery tank. 29 in.
- a twelfth valve 26 may be disposed between the first check valve 27 and the recovery tank 29. When the carbon disulfide needs to be injected into the adsorption tank, the twelfth valve 26 may be closed, so that the carbon disulfide liquid in the liquefaction tank 25 flows to the injection. In the liquid pump 28.
- the liquid injection pump 28 is in communication with the third opening of the canister 23.
- a thirteenth valve 31 may be disposed between the liquid injection pump 28 and the third opening of the adsorption tank 23, and when it is necessary to inject carbon disulfide into the adsorption tank 23, the thirteenth valve 31 is opened, and the liquid injection pump 28 injects carbon disulfide into the liquefaction.
- the tank 25 Inside the tank 25.
- the eleventh valve 24 may be disposed on the pipeline leading to the fourteenth valve 32 and the thirteenth valve 31 by the liquid injection pump 28.
- the eleventh valve 24 can be used as a total control valve to open the eleventh valve 24, and the carbon disulfide liquid can flow into the collection tank 35 through the fourteenth valve 32, or the infusion pump 28 can flow into the adsorption tank through the thirteenth valve 31. twenty three.
- the infusion pump 28 is connectable between the sampler 8 and the first inlet of the control valve 20.
- a second check valve 30 may be disposed on the line between the first pump 6 and the first inlet of the control valve 20, such that the second check valve 30, the ninth valve 14 and the first valve are opened.
- the ten valve 15, the carbon disulfide liquid in the liquid injection pump 28 flows through the second filter 16 and the third filter 17, to clean impurities or elemental sulfur remaining in the pipeline to avoid blockage of the pipeline.
- This embodiment provides a method for determining the solubility of elemental sulfur in a sulfur-containing gas.
- the implementation of the method is based on an experimental device.
- the layout of the experimental device is as shown in FIG. 1 , including a high temperature chamber 2 and a sample preparation device. 3.
- the outlet of the sampler 3 is in communication with the inlet of the back pressure valve 4, the outlet of the back pressure valve 4 is in communication with the inlet of the adsorption tank 6, and the first outlet of the adsorption tank 6 is in communication with the flow meter 7;
- the sampler 3 is located in the high temperature tank 2, the adsorption tank 6 is located in the low temperature tank 5, and a valve 10 is provided between the outlet of the sampler 2 and the inlet of the back pressure valve 3, and the collection tank 9 is adapted to be heated.
- the method for measuring the solubility of elemental sulfur in the sulfur-containing gas is as shown in FIG. 3, and includes steps S101 to S108. Each step will be specifically described below.
- S101 Collecting a sulfur-containing gas in a sulfur-containing gas reservoir, and measuring a sampling temperature and a sampling pressure when the sulfur-containing gas is collected.
- the experimental apparatus further includes a sampling cylinder 1, and the outlet of the sampling cylinder 1 is connected to the inlet of the sampler.
- Sampling cylinder 1 can be used to collect sulfur-containing gas in sulfur-containing gas reservoirs, and the sampling pressure and sampling temperature when collecting sulfur-containing gas are measured by a pressure gauge and a thermometer.
- S102 Transfer the sulfur-containing gas into the sampler, so that the sampler swings at a preset temperature and a preset pressure for a preset length of time.
- the elemental sulfur portion dissolved in the sulfur-containing gas may be analyzed due to changes in temperature and pressure.
- the sulfur-containing gas is first transferred into the sampler located in the high temperature chamber, and the preset time is swayed to prevent elemental sulfur from being precipitated.
- the preset temperature, preset pressure and preset duration can be set according to actual conditions.
- the preset temperature can be 80 ° C
- the preset pressure can be 1 MPa
- the preset duration can be 24 hours.
- the gas flow rate is too large, and the sulfur element in the gas is not sufficiently adsorbed in the carbon disulfide liquid, the gas is firstly balanced and depressurized through the back pressure valve 4, and the gas is stabilized.
- the ground flows out of the back pressure valve 4 and enters the adsorption tank 6.
- S104 The gas flowing out of the adsorption tank is passed through a gas flow meter, and the gas flow meter measures the volume of the sulfur-containing gas at room temperature and room pressure.
- a gas flow meter of a suitable range should be selected.
- room temperature and chamber pressure refer to the temperature of the laboratory in which the laboratory and the experimental apparatus are placed.
- S105 Collect and transfer the carbon disulfide liquid in the adsorption tank to the collection tank.
- the lower end of the adsorption tank 6 may be provided with a second outlet, and the second outlet of the adsorption tank 6 is connected to the collection tank 9 through a pipeline, and the adsorption tank 6 A valve 11 is provided on the line between the tank and the collection tank 9.
- the valve 11 is opened, and the carbon disulfide liquid in the adsorption tank 6 flows into the collection tank 9 through the pipeline, which is convenient to operate.
- S106 cooling the collecting tank and cooling, and measuring the mass of elemental sulfur in the collecting tank.
- the carbon disulfide liquid in the collection tank is converted into a gas and volatilized, and the elemental sulfur remains in the collection tank.
- the mass of elemental sulfur in the collection tank is determined, that is, the mass of elemental sulfur dissolved in the sulfur-containing gas.
- the pressure of the gas measured by the flow meter is the pressure at room temperature and chamber pressure.
- the room temperature and the chamber pressure are measured using a thermometer and a pressure gauge.
- S108 Calculating the solubility of elemental sulfur in the sulfur-containing gas according to the sampling temperature, the sampling pressure, the room temperature, the chamber pressure, the mass of the elemental sulfur, and the volume of the sulfur-containing gas at room temperature and the chamber pressure.
- this step includes sub-steps S1081, S1082, and S1083. The details are described below.
- S1081 Calculate the volume of the sulfur-containing gas in the standard state according to the room temperature, the chamber pressure and the volume of the sulfur-containing gas at room temperature and room pressure. The calculation formula is:
- V 0 the volume of the sulfur-containing gas in the state of the standard
- V 1 the volume of sulfur-containing gas at room temperature and chamber pressure
- the pressure in the nominal state is one atmosphere, and the temperature in the standard state is 20 °C.
- S1082 Calculate the volume of the sulfur-containing gas at the sampling temperature and the sampling pressure according to the volume, sampling temperature and sampling pressure of the sulfur-containing gas in the standard state, and the calculation formula is:
- V' 1 the volume of the sulfur-containing gas at the sampling temperature and the sampling pressure
- V 0 the volume of the sulfur-containing gas in the state of the standard
- T sampling temperature
- the deviation factor Z of the gas at the sampling temperature and the sampling pressure can be obtained by a gas phase experiment.
- S1083 Calculate the solubility of the elemental sulfur of the sulfur-containing gas according to the volume of the sulfur-containing gas at the sampling temperature and the sampling pressure and the mass of the elemental sulfur, and the calculation formula is:
- V' 1 the volume of the sulfur-containing gas at the sampling temperature and sampling pressure.
- the exhaust gas absorption tank 8 is connected to the outlet of the flow meter 7.
- the exhaust gas absorption tank 8 adsorbs harmful gases in the gas to prevent contamination of the environment.
- the solubility c i of the elemental sulfur of the corresponding sulfur-containing gas at different sampling temperatures and sampling pressures is obtained by changing the sampling temperature and the sampling pressure.
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Abstract
一种含硫气体中的元素硫溶解度的测定装置及方法，其中，该装置包括驱替泵（1）、第一取样器（6）、高温箱（18）、回压泵（21）、控制阀（20）、吸附罐（23）、低温箱（48）、流量计和收集罐（35），其中，所述驱替泵（1）的出口与所述第一取样器（6）的进口连通，所述第一取样器（6）的出口与所述控制阀（20）的第一进口连通，所述控制阀（20）的第二进口与所述回压泵（21）的出口连通，所述控制阀（20）的出口与所述吸附罐（23）的第一开口连通，所述吸附罐（23）的第二开口与所述流量计连通；所述吸附罐（23）的第三开口与所述收集罐（35）连通；所述第一取样器（6）位于所述高温箱（18）内，所述吸附罐（23）位于所述低温箱（48）内，所述第一取样器（6）的出口与所述控制阀（20）的第一进口之间设置有阀门（7），所述吸附罐（23）的第三开口与所述收集罐（35）之间设置有阀门（32），所述收集罐（35）适于被加热。
Description
本发明涉及一种含硫气体中的元素硫溶解度的测定装置及方法，属于油气开采技术领域。
与常规气藏开发相比，高含硫气藏中存在元素硫的溶解和沉积作用。当压力和温度降低时，元素硫在高含硫气体中的溶解度会下降。当气体中硫含量大于硫的溶解度时，元素硫就会沉积下来。沉积的元素硫不仅会堵塞地层，极大地降低地层渗透率，严重影响气井产能，而且还会给气井的正常生产、输送和管理带来危害。因此，有必要准确地测定和计算元素硫在高含硫气藏流体中的溶解度，为高含硫气藏合理开发、产能配产、方案制定以及下游集输设计提供重要的基础和依据。
国内关于含硫饱和度(含硫气体中的元素硫溶解度)的研究，大多是基于理论和模型研究，无法保证研究结果的精确性。目前还没有相关的可以精确测定含硫气体中的元素硫溶解度的实验装置及方法。
发明内容
为解决上述技术问题，本发明的目的在于提供一种含硫气体中的元素硫溶解度的测定装置。
本发明的目的还在于提供一种含硫气体中的元素硫溶解度的测定方法。
为达到上述目的，一方面，本发明提供一种含硫气体中的元素硫溶解度的测定装置，该装置包括驱替泵、第一取样器、高温箱、回压泵、控制阀、吸附罐、低温箱、流量计和收集罐，其中，所述驱替泵的出口与所述第一取样器的进口连通，所述第一取样器的出口与所述控制阀的第一进口连通，所述控制阀的第二进口与所述回压泵的出口连通，所述控制阀的出口与所述吸附罐的第一开口连通，所述吸附罐的第二开口与所述流量计连通；所述吸附罐的第三开口与所述收集罐连通；
所述第一取样器位于所述高温箱内，所述吸附罐位于所述低温箱内，所述第一取样器的出口与所述控制阀的第一进口之间设置有阀门，所述吸附罐的第三开口与所述 收集罐之间设置有阀门，所述收集罐适于被加热。
根据本发明所述的装置，优选地，所述装置还包括配样器，所述第一取样器的出口与所述配样器的进口连通，所述配样器的出口与所述控制阀的第一进口连通，所述配样器位于所述高温箱内。
根据本发明所述的装置，进一步地，若所述配样器中盛装有硫粉，则此时所述装置还包括摇摆装置，该摇摆装置与所述配样器相连接。
其中，所述摇摆装置为本领域使用的常规装置且其与配样器之间的连接也为本领域常规连接，本申请所提供的该装置安装该摇摆装置的目的为使配样器在恒温恒压的状态下进行摇摆。
根据本发明所述的装置，优选地，所述配样器的出口与所述控制阀的第一进口之间设置有过滤器。
根据本发明所述的装置，优选地，所述装置还包括第二取样器，所述第二取样器的进口与所述驱替泵连通，所述第二取样器的出口与所述控制阀的第一进口连通。
根据本发明所述的装置，优选地，所述第二取样器与所述控制阀的第一进口之间设置有过滤器。
根据本发明所述的装置，优选地，所述控制阀的出口与所述吸附罐的第一开口之间设置有第一盘管，所述第一盘管位于所述低温箱内。
根据本发明所述的装置，优选地，所述吸附罐的第二开口与所述流量计之间设置有第二盘管。
根据本发明所述的装置，优选地，所述流量计为至少两个，所述至少两个流量计并联后连接在所述第二盘管之后，每个流量计与所述第二盘管之间均连通有气动阀。
根据本发明所述的装置，优选地，所述流量计的出口与尾气处理罐连通。
根据本发明所述的装置，优选地，所述装置还包括液化罐，所述液化罐位于所述低温箱内，所述收集罐与所述液化罐的进口连通，所述收集罐与所述液化罐之间的管路上设置有可从所述收集罐流向所述液化罐的单向阀。
根据本发明所述的装置，优选地，所述装置还包括回收罐和注液泵，所述回收罐和所述注液泵分别与所述液化罐的出口连通。
根据本发明所述的装置，优选地，所述注液泵与所述吸附罐的第三开口连通。
根据本发明所述的装置，优选地，所述注液泵连接到所述配样器与所述控制阀的 第一进口之间。
本发明还提供了一种含硫气体中的元素硫溶解度的测定方法，以比较准确地得到含硫气体中的元素硫溶解度。
具体而言，包括以下的技术方案：
采集含硫气藏中的含硫气体，测定采集所述含硫气体时的取样温度和取样压力；
将所述含硫气体转入配样器中，使所述配样器在预设温度及预设压力下摇摆预设时长；
打开所述配样器出口端阀门，使所述配样器内的气体通过回压阀后压力降至室压，之后流入吸附罐内，其中所述吸附罐内盛放二硫化碳液体；
从所述吸附罐流出的气体通过气体流量计，所述气体流量计测定所述含硫气体在室温和所述室压下的体积；
将所述吸附罐内的二硫化碳液体收集并转移到收集罐内；
加热所述收集罐后冷却，测定所述收集罐内的元素硫的质量；
测定所述室温和所述室压；
根据所述取样温度、所述取样压力、所述室温、所述室压、所述元素硫的质量及所述含硫气体在所述室温和所述室压下的体积，计算得到所述含硫气体中元素硫的溶解度；
其中，所述配样器的出口与所述回压阀的进口连通，所述回压阀的出口与所述吸附罐的进口连通，所述吸附罐的第一出口与所述流量计连通；
所述配样器位于所述高温箱内，所述吸附罐位于所述低温箱内，所述配样器的出口与所述回压阀的进口之间设置有阀门，所述收集罐适于被加热。
可选择地，所述根据所述取样温度、所述取样压力、所述室温、所述室压、所述元素硫的质量及所述含硫气体在所述室温和所述室压下的体积，计算得到所述含硫气体中元素硫的溶解度，包括：
根据所述室温、所述室压及所述含硫气体在所述室温和所述室压下的体积，计算得到所述含硫气体在标态下的体积；
根据所述含硫气体在标态下的体积、所述取样温度及所述取样压力，计算得到所述含硫气体在所述取样温度和所述取样压力下的体积；
根据所述含硫气体在所述取样温度和所述取样压力下的体积及所述元素硫的质 量，计算得到所述含硫气体中的元素硫的溶解度。
可选择地，所述根据所述室温、所述室压及所述含硫气体在所述室温和所述室压下的体积，计算得到所述含硫气体在标态下的体积，采用的计算公式如下：
式中，
V
0——含硫气体在标态下的体积；
P
0——标态下的压力；
T
0——标态下的温度；
P
1——室压；
V
1——含硫气体在室温和室压下的体积；
T
1——室温。
可选择地，所述根据含硫气体在标态下的体积、所述取样温度及所述取样压力，计算得到所述含硫气体在所述取样温度和所述取样压力下的体积，采用的计算公式为：
式中，
V′
1——含硫气体在取样温度和取样压力下的体积；
P
0——标态下的压力；
V
0——含硫气体在标态下的体积；
T
0——标态下的温度；
P——取样压力；
T——取样温度；
Z——气体在取样温度和取样压力下的偏差因子。
可选择地，所述根据含硫气体在所述取样温度和所述取样压力下的体积及所述元素硫的质量，计算得到所述含硫气体中元素硫的溶解度，采用的计算公式为：
式中，
c——含硫气体中元素硫的溶解度；
m——元素硫的质量；
V′
1——含硫气体在取样温度和取样压力下的体积。
可选择地，在所述加热所述收集罐后冷却，测定所述收集罐内的元素硫的质量之前，所述方法还包括：
采用二硫化碳液体清洗所述配样器与所述吸附罐之间的管线，将清洗后的二硫化碳液体收集并转移到所述收集罐内。
可选择地，所述气体流量计的出口连接有尾气吸收罐。
可选择地，所述吸附罐的下端开设有第二出口，所述吸附罐的所述第二出口与所述收集罐通过管线连接，所述吸附罐和所述收集罐之间的管线上设置有阀门。
另一方面，本发明还提供了一种含硫气体中的元素硫溶解度的测定方法，其包括：
(1)采集含硫气藏中的含硫气体，测定采集所述含硫气体时的取样温度和取样压力；
(2)使步骤(1)中的含硫气体平衡降压至室压，再采用二硫化碳液体吸附该含硫气体；
(3)测量步骤(2)吸附后所得含硫气体在室温和所述室压下的体积；
(4)加热步骤(3)中得到的吸附元素硫后的二硫化碳液体以除去二硫化碳，称量所得元素硫的质量；
(5)根据所述取样温度、所述取样压力、所述室温、所述室压、所述元素硫的质量及步骤(2)吸附后所得含硫气体在所述室温和所述室压下的体积，计算得到所述含硫气体中元素硫的溶解度。
根据本发明所述的方法，优选地，步骤(5)所述根据所述取样温度、所述取样压力、所述室温、所述室压、所述元素硫的质量及步骤(2)吸附后所得含硫气体在所述室温和所述室压下的体积，计算得到所述含硫气体中元素硫的溶解度，包括：
根据所述室温、所述室压及步骤(2)吸附后所得含硫气体在所述室温和所述室压下的体积，计算得到所述含硫气体在标态下的体积；
根据所述含硫气体在标态下的体积、所述取样温度及所述取样压力，计算得到所述含硫气体在所述取样温度和所述取样压力下的体积；
根据所述含硫气体在所述取样温度和所述取样压力下的体积及所述元素硫的质量，计算得到所述含硫气体中的元素硫的溶解度。
根据本发明所述的方法，优选地，所述根据所述室温、所述室压及步骤(2)吸附后所得含硫气体在所述室温和所述室压下的体积，计算得到所述含硫气体在标态下的体积包括采用如下式(1)计算得到所述含硫气体在标态下的体积；
式(1)中，
V
0——含硫气体在标态下的体积；
P
0——标态下的压力；
T
0——标态下的温度；
P
1——室压；
V
1——含硫气体在室温和室压下的体积；
T
1——室温。
根据本发明所述的方法，优选地，所述根据所述含硫气体在标态下的体积、所述取样温度及所述取样压力，计算得到所述含硫气体在所述取样温度和所述取样压力下的体积包括采用如下式(2)计算得到所述含硫气体在所述取样温度和所述取样压力下的体积；
式(2)中，
V′
1——含硫气体在取样温度和取样压力下的体积；
P
0——标态下的压力；
V
0——含硫气体在标态下的体积；
T
0——标态下的温度；
P——取样压力；
T——取样温度；
Z——气体在取样温度和取样压力下的偏差因子。
根据本发明所述的方法，优选地，所述根据所述含硫气体在所述取样温度和所述 取样压力下的体积及所述元素硫的质量，计算得到所述含硫气体中的元素硫的溶解度包括采用如下式(3)计算得到所述含硫气体中的元素硫的溶解度；
式(3)中，
c——含硫气体中元素硫的溶解度；
m——元素硫的质量；
V′
1——含硫气体在取样温度和取样压力下的体积。
根据本发明所述的方法，优选地，该方法具体包括以下步骤：
(1)采集含硫气藏中的含硫气体，测定采集所述含硫气体时的取样温度和取样压力；
(2)将所述含硫气体转入配样器中，使所述配样器在预设温度及预设压力下摇摆预设时长，以防止含硫气体中的元素硫析出；
(3)使步骤(2)中的含硫气体平衡降压至室压，之后流入吸附罐内，其中，所述吸附罐内盛放二硫化碳液体；
(4)从所述吸附罐流出的气体通过气体流量计，所述气体流量计测定步骤(3)所得含硫气体在室温和所述室压下的体积；
(5)将所述吸附罐内的二硫化碳液体收集并转移到收集罐内；加热所述收集罐以除去二硫化碳，冷却，测定所述收集罐内的元素硫的质量；
(6)根据所述取样温度、所述取样压力、所述室温、所述室压、所述元素硫的质量及步骤(3)所得含硫气体在室温和所述室压下的体积，计算得到所述含硫气体中元素硫的溶解度。
根据本发明所述的方法，优选地，在所述步骤(5)之前，该方法还包括：
采用二硫化碳液体清洗所述配样器与所述吸附罐之间的管线，再将清洗后的二硫化碳液体收集并转移到所述收集罐内。
本发明所提供的含硫气体中的元素硫溶解度的测定方法及装置可以通过驱替泵将第一取样器中的含硫气体驱替到控制阀，通过调节回压泵的压力，使气体经控制阀实现平衡降压并平稳流出，从而可保证流量计测得的气体流量比较准确；第一取样器位于高温箱内，可避免气体中的元素硫析出，保证测量结果准确；吸附罐位于低温箱 中，可保证气体中的元素硫在吸附罐中吸附比较充分；加热收集罐可得到气体中的元素硫的含量。因此基于本发明提供的装置及方法测得的气体中元素硫的含量比较准确，进而基于该装置及方法测得的气体流量及气体中元素硫的含量，计算得到含硫气体中的元素硫的溶解度比较精确。
图1为本发明其一实施方式所提供的含硫气体中的元素硫溶解度的测定装置的结构示意图；
图2为本发明另一实施方式所提供的含硫气体中的元素硫溶解度的测定装置的结构示意图；
图3为本发明实施例所提供的含硫气体中的元素硫溶解度的测定方法工艺流程图。
主要附图标号说明：
图1中：
1、取样钢瓶；2、高温箱；3、配样器；4、回压阀；5、低温箱；6、吸附罐；7、气体流量计；8、尾气吸收罐；9、收集罐；10、阀门；11、阀门。
图2中：
1、驱替泵；2、第一阀门；3、第二阀门；4、第三阀门；5、第四阀门；6、第一取样器；7、第五阀门；8、配样器；9、第六阀门；10、第七阀门；11、第二取样器；12、第一过滤器；13、第八阀门；14、第九阀门；15、第十阀门；16、第二过滤器；17、第三过滤器；18、高温箱；19、紧急制动阀；20、控制阀；21、回压泵；22、第一盘管；23、吸附罐；24、第十一阀门；25、液化罐；26、第十二阀门；27、第一单向阀；28、注液泵；29、回收罐；30、第二单向阀；31、第十三阀门；32、第十四阀门；33、第三单向阀；34、第十五阀门；35、收集罐；36、第二盘管；37、第一气动阀；38、第一流量计；39、第二气动阀；40、第二流量计；41、第三气动阀；42、第三流量计；43、第十六阀门；44、第四单向阀；45、第五单向阀；46、尾气处理罐；47、第六单向阀；48、低温箱。
为了对本发明的技术特征、目的和有益效果有更加清楚的理解，以下将通过具体 的实施例及说明书附图详细地说明本发明的实施过程和产生的有益效果，旨在帮助阅读者更好地理解本发明的实质和特点，但是不作为对本案可实施范围的限定。
实施例1
本实施例提供了一种含硫气体中的元素硫溶解度的测定装置，其包括驱替泵1、第一取样器6、高温箱18、回压泵21、控制阀20、吸附罐23、低温箱48、流量计和收集罐35，其中，
驱替泵1的出口与第一取样器6的进口连通，第一取样器6的出口与控制阀20的第一进口连通，控制阀20的第二进口与回压泵21的出口连通，控制阀20的出口与吸附罐23的第一开口连通，吸附罐23的第二开口与流量计连通；吸附罐23的第三开口与收集罐35连通；
第一取样器6位于高温箱18内，吸附罐23位于低温箱48内，第一取样器6的出口与控制阀20的第一进口之间设置有第五阀门7，吸附罐23的第三开口与收集罐35之间设置有第十四阀门32，收集罐35适于被加热。
在本实施例中，相邻的器件之间的连通可通过管路来实现，但本发明不限于此，也可采用直接相连或其他方式实现。在本申请中，描述一个器件与另一个器件连通时，意指两者可通过管路、直接相连或其他合适的方式来达到连通。
使用本实施例提供的装置时，首先将待测气体放到第一取样器6中，先将第六阀门9关闭，打开回压泵21，使回压泵21内的水从控制阀20的第二进口进入，然后打开第六阀门9，使待测气体从控制阀20的第一进口进入，接着调节回压泵21的压力，使经过控制阀20的气体的压力与回压泵21的回压的压力差在0.1MPa的范围内，从而使气体经控制阀20实现平衡降压，进而气体平稳地从控制阀20流出并进入到吸附罐23内。在吸附罐23中，吸附罐23内的二硫化碳液体对含硫气体中的元素硫进行吸附。从吸附罐23流出的气体进入到流量计，流量计可测出气体的体积。接下来打开吸附罐23与收集罐35之间的第十四阀门32，吸附罐23中的二硫化碳液体流入到收集罐35中，然后对收集罐35进行加热，二硫化碳变成气体挥发，而元素硫留在收集罐35中，称量即可得到元素硫的质量。最后，根据元素硫的质量、气体的流量，结合模型即可计算出高含硫气体中的元素硫的溶解度。在该装置中，第一采样器6位于高温箱18内可保证气体中的元素硫不会析出；并且吸附罐23位于低温箱48内，可以保证吸附罐23中的二硫化碳液体不会挥发，而元素硫在吸附罐23内吸附比较充 分，因此本发明提供的装置可比较精确地测得气体中的元素硫的溶解度。
在本实施例中，高温箱18可以是空气浴高温箱，也可以是其他形式的高温箱。
实施例2
本实施例提供了一种含硫气体中的元素硫溶解度的测定装置，该装置的结构示意图如图2所示，从图2中可以看出，在实施例1所提供装置的基础上，本实施例的该装置还包括配样器8和摇摆装置，第一取样器6的进口与驱替泵1的出口连通，第一取样器6的出口与配样器8的进口连通，配样器8的出口与控制阀20的第一进口连通，配样器8位于高温箱18内，与摇摆装置连接。在配样器8与控制阀20之间设置有第六阀门9，第一取样器6与配样器8之间设置有第五阀门7和第七阀门10，第一取样器6与驱替泵1之间设置有第二阀门3。在该情况下，如图2所示，由于高温箱18的体积受限，第一取样器6可置于高温箱18外，需要测第一取样器6内气体中元素硫的溶解度时，将第一取样器6中的气体驱替到高温箱18内的配样器8内即可。当需要测定饱和含硫气体中元素硫的溶解度时，关闭第六阀门9，打开第二阀门3、第五阀门7和第七阀门10，驱替泵1将第一取样器6中的气体驱替到配样器8中，然后再关闭第二阀门3、第五阀门7和第七阀门10。在配样器8中放置有过量的硫粉，打开摇摆装置，使配样器8在恒温恒压的状态摇摆24小时，保证饱和含硫气体中的元素硫不会析出。在配样器8与驱替泵1的出口之间设置有第三阀门4，打开第三阀门4，驱替泵1驱使配样器8中的饱和含硫气体从控制阀20的第一进口进入，调节回压泵21的压力，使饱和含硫气体经控制阀20实现平衡降压后并平稳流入到吸附罐中。
如图2所示，在驱替泵1与配样器8之间的管路上设置有支路，支路上设置有第四阀门5，第四阀门5用来排出配样器8内的水。
如图2所示，在控制阀20的第一进口与配样器8及第一取样器6之间可设置有紧急制动阀19，即紧急制动阀19可同时制止配样器8到控制阀20的第一进口的流通。当气体的流量过大超过流量计的量程时，可关闭紧急制动阀19，避免造成流量计的损坏。
在本实施例中，如图2所示，配样器8的出口与控制阀20的第一进口之间设置有第二过滤器16。第二过滤器16可将从配样器8中流出的气体中的酸液、沥青及胶质等过滤掉，避免造成管路的堵塞。为了使过滤效果更好，第二过滤器16和第三过 滤器17可并联后连通到配样器8与控制阀20之间。配样器8与第二过滤器16之间设置有第九阀门14，配样器8与第三过滤器17之间设置有第十阀门15。打开第九阀门14和第十阀门15，配样器8中的气体分别通过第二过滤器16和第三过滤器17，再流入控制阀20。
在本实施例中，如图2所示，所述装置还包括第二取样器11，第二取样器11的进口与驱替泵1连通，第二取样器11的出口与控制阀20的第一进口连通。第二取样器11可为井下取样器，从井下取出的气体样品压力较大，直接经控制阀20实现平衡降压。在本实施例中，如图2所示，第二取样器11与控制阀20的第一进口之间设置有第一过滤器12。第一过滤器12可将从第二取样器11中流出的气体中的酸液、沥青及胶质等过滤掉，避免造成管路的堵塞。
如图2所示，驱替泵1与第二取样器11之间设置有第一阀门2，第二取样器11与控制阀20之间设置有第八阀门13。打开第一阀门2和第八阀门13，驱替泵1驱使第二取样器11中的气体流经控制阀20。在本实施例中，如图2所示，控制阀20的出口与吸附罐23的进口之间设置有第一盘管22，第一盘管22位于低温箱48内。从控制阀20流出的气体可先在第一盘管22中实现降温，再进入到吸附罐23中，避免进入吸附罐23中的气体温度太高造成二硫化碳挥发。
在本实施例中，如图2所示，吸附罐23的第二开口与流量计之间设置有第二盘管36。从吸附罐23流出的气体可先经第二盘管36降低气速，避免气体气速过高造成流量计超量程。
在本实施例中，如图2所示，流量计为三个，三个流量计并联后连通在第二盘管36之后，每个流量计与第二盘管36之间均连通有气动阀。如图2所示，第一流量计38与第一气动阀37串联，第二流量计40与第二气动阀39串联，第三流量计42与第三气动阀41串联。三个流量计的量程不同，可根据需要选择合适量程的流量计，从而保证测得的气体流量更准确。通过控制第一气动阀37、第二气动阀39及第三气动阀41使气体进入指定的流量计。本实施例以流量计的数量为三个进行说明，但本发明不限于此。
在本实施例中，如图2所示，流量计的出口与尾气处理罐46连通。尾气处理罐46与流量计之间设置有第四单向阀44，当有气体从流量计的出口流出时，打开第四单向阀44，从而气体可进入到尾气处理罐46中，防止污染环境。尾气处理罐46的 出口管路上设置有第六单向阀47。打开第六单向阀47，经尾气处理罐46处理后的气体可流入其他装置。
在本实施例中，如图2所示，所述装置还包括液化罐25，液化罐25位于低温箱48内，收集罐35与液化罐25的进口连通，收集罐35与液化罐25之间的管路上设置有可从收集罐35流向液化罐25的第三单向阀33。与收集罐35内连通的管路上设置有第十五阀门34，加热收集罐35时，打开第十五阀门34并注入干燥的且不与元素硫及二硫化碳发生反应的惰性气体，比如氮气，惰性气体将收集罐35内的二硫化碳气体全部从收集罐35内带出并进入液化罐25内。进入液化罐25内的二硫化碳气体液化并沉积到液化罐25的下部。液化罐25的上端的出口与尾气处理罐46之间设置有第十六阀门43，打开第十六阀门43，惰性气体从液化罐25的上端排出并进入到尾气处理罐46。液化罐25的上端的出口通过管路连接到第五单向阀45前，此时需要在第五单向阀45与流量计之间设置第四单向阀44，打开第十六阀门43时需关闭第四单向阀44，防止惰性气体回流到流量计中。
在本实施例中，如图2所示，所述装置还包括回收罐29和注液泵28，回收罐29和注液泵28分别与液化罐25的出口连通。在液化罐25通向回收罐29和注液泵28的管路上设置有第一单向阀27，打开第一单向阀27，液化罐25内的二硫化碳液体流到注液泵28和回收罐29中。可在第一单向阀27与回收罐29之间设置第十二阀门26，当需要向吸附罐中注入二硫化碳时，可关闭第十二阀门26，从而液化罐25内的二硫化碳液体流到注液泵28中。
在本实施例中，如图2所示，注液泵28与吸附罐23的第三开口连通。可在注液泵28与吸附罐23的第三开口之间设置第十三阀门31，当需要向吸附罐23内注入二硫化碳时，打开第十三阀门31，注液泵28将二硫化碳注入到液化罐25内。
如图2所示，注液泵28通向第十四阀门32及第十三阀门31的管路上可设置有第十一阀门24。第十一阀门24可作为总的控制阀，打开第十一阀门24，二硫化碳液体才能经第十四阀门32流入到收集罐35，或者注液泵28才能经第十三阀门31流入到吸附罐23。
在本实施例中，如图2所示，注液泵28可连通到配样器8与控制阀20的第一进口之间。在注液泵28通向第一取样器6与控制阀20的第一进口之间的管路上可设置第二单向阀30，这样，打开第二单向阀30、第九阀门14和第十阀门15，注液泵28 内的二硫化碳液体流经第二过滤器16和第三过滤器17，清洗残留在管路中的杂质或者元素硫，避免管路堵塞。
在图1及图2中，箭头代表管路中气体或者液体的流动方向。
实施例3
本实施例提供了一种含硫气体中的元素硫溶解度的测定方法，该方法的实现是基于实验装置实现的，实验装置的平面布置图如图1所示，包括高温箱2、配样器3、回压阀4、低温箱5、吸附罐6、流量计7和收集罐9；
其中，配样器3的出口与回压阀4的进口连通，回压阀4的出口与吸附罐6的进口连通，吸附罐6的第一出口与流量计7连通；
配样器3位于高温箱2内，吸附罐6位于低温箱5内，配样器2的出口与回压阀3的进口之间设置有阀门10，收集罐9适于被加热。
含硫气体中的元素硫溶解度的测定方法如图3所示，包括步骤S101-S108。下面将对各步骤进行具体说明。
S101：采集含硫气藏中的含硫气体，测定采集含硫气体时的取样温度和取样压力。
如图1所示，实验装置还包括取样钢瓶1，取样钢瓶1的出口与配样器的进口连接。可采用取样钢瓶1采集含硫气藏中的含硫气体，并采用压力计和温度计测得采集含硫气体时的取样压力和取样温度。
S102：将含硫气体转入配样器中，使配样器在预设温度及预设压力下摇摆预设时长。
从气藏中采集含硫气体样品后，可能会因为温度和压力的变化导致含硫气体中溶解的元素硫部分析出。为了保证实验的准确性，先将含硫气体转入位于高温箱中的配样器中，并摇摆预设时长，防止元素硫析出。预设温度、预设压力和预设时长可根据实际情况设定，例如，预设温度可为80℃，预设压力可为1MPa，预设时长可为24小时。
S103：打开配样器出口端阀门，使配样器内的气体通过回压阀后压力降至室压，之后流入吸附罐内，其中吸附罐内盛放二硫化碳液体。
为了防止从配样器流出的气体压力太大导致气体流速过大，进而造成气体中的硫单质在二硫化碳液体中吸附不充分的情况，先使气体通过回压阀4平衡降压，进而气体平稳地从回压阀4流出并进入到吸附罐6内。
S104：从吸附罐流出的气体通过气体流量计，气体流量计测定含硫气体在室温和室压下的体积。
其中，为了保证气体体积测定的准确性，应选择合适量程的气体流量计。
在本实施例中，室温和室压指的是进行实验室，实验装置所在的实验室的温度。
S105：将吸附罐内的二硫化碳液体收集并转移到收集罐内。
为了便于将吸附罐内的二硫化碳转移至收集罐内，如图1所示，吸附罐6的下端可开设有第二出口，吸附罐6的第二出口与收集罐9通过管线连接，吸附罐6和收集罐9之间的管线上设置有阀门11。
当含硫气体在吸附罐6内完成吸附后，打开阀门11，吸附罐6内的二硫化碳液体即通过管线流入到收集罐9内，操作比较方便。
S106：加热收集罐后冷却，测定收集罐内的元素硫的质量。
加热收集罐，则收集罐内的二硫化碳液体转化为气体并挥发，元素硫留在收集罐内。待收集罐冷却后，测定收集罐内的元素硫的质量，即为含硫气体中溶解的元素硫的质量。
S107：测定室温和室压。
流量计测得的气体的压力是在室温和室压下的压力，为了便于后续计算，采用温度计和压力计测定室温和室压。
S108：根据取样温度、取样压力、室温、室压、元素硫的质量及含硫气体在室温和室压下的体积，计算得到含硫气体中元素硫的溶解度。
具体地，该步骤包括子步骤S1081、S1082和S1083。下面进行详细介绍。
S1081：根据室温、室压及含硫气体在室温和室压下的体积，计算得到含硫气体在标态下的体积，采用的计算公式为：
式中，
V
0——含硫气体在标态下的体积；
P
0——标态下的压力；
T
0——标态下的温度；
P
1——室压；
V
1——含硫气体在室温和室压下的体积；
T
1——室温。
标态下的压力为一个大气压，标态下的温度为20℃。
S1082：根据含硫气体在标态下的体积、取样温度及取样压力，计算得到含硫气体在取样温度和取样压力下的体积，采用的计算公式为：
式中，
V′
1——含硫气体在取样温度和取样压力下的体积；
P
0——标态下的压力；
V
0——含硫气体在标态下的体积；
T
0——标态下的温度；
P——取样压力；
T——取样温度；
Z——气体在取样温度和取样压力下的偏差因子。
其中，气体在取样温度和取样压力下的偏差因子Z通过气体常规相态实验即可得到。
S1083：根据含硫气体在取样温度和取样压力下的体积及元素硫的质量，计算得到含硫气体的元素硫的溶解度，采用的计算公式为：
式中，
c——含硫气体中元素硫的溶解度；
m——元素硫的质量；
V′
1——含硫气体在取样温度和取样压力下的体积。
在采用实验装置进行实验时，含硫气体从回压阀流到吸附罐的过程中，可能会有很少量的元素硫残留在回压阀4与吸附罐6之间的管线上，为了提高实验的精确度，在实验结束后，可采用二硫化碳液体清洗配样器3与吸附罐6之间的管线，并将清洗后的二硫化碳液体收集并转移到回收罐9内，从而最后测得的元素硫的质量更精确。
为了防止气体污染环境，如图1所示，流量计7的出口连接有尾气吸收罐8。这 样，尾气吸收罐8将气体中的有害气体吸附，防止污染环境。
作为本发明的一种改进，对于同一气井，通过改变取样温度及取样压力，得到不同取样温度和取样压力条件下对应的含硫气体的元素硫的溶解度c
i。
根据Chrastil方程：
式中，
c——固体溶质在流体中的溶解度；
d——流体密度；
T——温度；
a，b，k——常数。
将Chrastil方程两边取对数，可得到：
令y＝lnc，x
1＝lnd，
则上式变形为：
y＝kx
1+ax
2+b；
将得到的c
i值代入变形后的公式，可求出a，b，k的值。从而确定取样温度及流体密度后，根据公式y＝kx
1+ax
2+b即可求出含硫气体中元素硫的溶解度，而无需通过实验，更加简单。
在本申请所提供的实施例中，应该理解到，术语“第一”、“第二”等仅用于描述目的，而不能理解为指示或暗示相对重要性或者隐含指明所指示的技术特征的数量。
以上所述仅是为了便于本领域的技术人员理解本发明的技术方案，并不用以限制本发明。凡在本发明的精神和原则之内，所作的任何修改、等同替换、改进等，均应包含在本发明的保护范围之内。
Claims (20)
- 一种含硫气体中的元素硫溶解度的测定装置，其特征在于，该装置包括驱替泵、第一取样器、高温箱、回压泵、控制阀、吸附罐、低温箱、流量计和收集罐，其中，所述驱替泵的出口与所述第一取样器的进口连通，所述第一取样器的出口与所述控制阀的第一进口连通，所述控制阀的第二进口与所述回压泵的出口连通，所述控制阀的出口与所述吸附罐的第一开口连通，所述吸附罐的第二开口与所述流量计连通；所述吸附罐的第三开口与所述收集罐连通；所述第一取样器位于所述高温箱内，所述吸附罐位于所述低温箱内，所述第一取样器的出口与所述控制阀的第一进口之间设置有阀门，所述吸附罐的第三开口与所述收集罐之间设置有阀门，所述收集罐适于被加热。
- 根据权利要求1所述的装置，其特征在于，所述装置还包括配样器，所述第一取样器的出口与所述配样器的进口连通，所述配样器的出口与所述控制阀的第一进口连通，所述配样器位于所述高温箱内。
- 根据权利要求2所述的装置，其特征在于，所述配样器的出口与所述控制阀的第一进口之间设置有过滤器。
- 根据权利要求1所述的装置，其特征在于，所述装置还包括第二取样器，所述第二取样器的进口与所述驱替泵连通，所述第二取样器的出口与所述控制阀的第一进口连通。
- 根据权利要求4所述的装置，其特征在于，所述第二取样器与所述控制阀的第一进口之间设置有过滤器。
- 根据权利要求1所述的装置，其特征在于，所述控制阀的出口与所述吸附罐的第一开口之间设置有第一盘管，所述第一盘管位于所述低温箱内。
- 根据权利要求1所述的装置，其特征在于，所述吸附罐的第二开口与所述流量计之间设置有第二盘管。
- 根据权利要求7所述的装置，其特征在于，所述流量计为至少两个，所述至少两个流量计并联后连接在所述第二盘管之后，每个流量计与所述第二盘管之间均连通有气动阀。
- 根据权利要求1所述的装置，其特征在于，所述流量计的出口与尾气处理罐连通。
- 根据权利要求1所述的装置，其特征在于，所述装置还包括液化罐，所述液化罐位于所述低温箱内，所述收集罐与所述液化罐的进口连通，所述收集罐与所述液化罐之间的管路上设置有从所述收集罐流向所述液化罐的单向阀。
- 根据权利要求10所述的装置，其特征在于，所述装置还包括回收罐和注液泵，所述回收罐和所述注液泵分别与所述液化罐的出口连通。
- 根据权利要求11所述的装置，其特征在于，所述注液泵与所述吸附罐的第三开口连通。
- 根据权利要求11所述的装置，其特征在于，所述注液泵连接到配样器与所述控制阀的第一进口之间。
- 一种含硫气体中的元素硫溶解度的测定方法，其特征在于，该方法包括：(1)采集含硫气藏中的含硫气体，测定采集所述含硫气体时的取样温度和取样压力；(2)使步骤(1)中的含硫气体平衡降压至室压，再采用二硫化碳液体吸附该含硫气体；(3)测量步骤(2)吸附后所得含硫气体在室温和所述室压下的体积；(4)加热步骤(3)中得到的吸附元素硫后的二硫化碳液体以除去二硫化碳，称量所得元素硫的质量；(5)根据所述取样温度、所述取样压力、所述室温、所述室压、所述元素硫的质量及步骤(2)吸附后所得含硫气体在所述室温和所述室压下的体积，计算得到所述含硫气体中元素硫的溶解度。
- 根据权利要求14所述的方法，其特征在于，步骤(5)所述根据所述取样温度、所述取样压力、所述室温、所述室压、所述元素硫的质量及步骤(2)吸附后所得含硫气体在所述室温和所述室压下的体积，计算得到所述含硫气体中元素硫的溶解度，包括：根据所述室温、所述室压及步骤(2)吸附后所得含硫气体在所述室温和所述室压下的体积，计算得到所述含硫气体在标态下的体积；根据所述含硫气体在标态下的体积、所述取样温度及所述取样压力，计算得到所述含硫气体在所述取样温度和所述取样压力下的体积；根据所述含硫气体在所述取样温度和所述取样压力下的体积及所述元素硫的质 量，计算得到所述含硫气体中的元素硫的溶解度。
- 根据权利要求15所述的方法，其特征在于，所述根据所述室温、所述室压及步骤(2)吸附后所得含硫气体在所述室温和所述室压下的体积，计算得到所述含硫气体在标态下的体积包括采用如下式(1)计算得到所述含硫气体在标态下的体积；
式(1)中，V 0——含硫气体在标态下的体积；P 0——标态下的压力；T 0——标态下的温度；P 1——室压；V 1——含硫气体在室温和室压下的体积；T 1——室温。 - 根据权利要求15所述的方法，其特征在于，所述根据所述含硫气体在标态下的体积、所述取样温度及所述取样压力，计算得到所述含硫气体在所述取样温度和所述取样压力下的体积包括采用如下式(2)计算得到所述含硫气体在所述取样温度和所述取样压力下的体积；
式(2)中，V 1'——含硫气体在取样温度和取样压力下的体积；P 0——标态下的压力；V 0——含硫气体在标态下的体积；T 0——标态下的温度；P——取样压力；T——取样温度；Z——气体在取样温度和取样压力下的偏差因子。 - 根据权利要求15所述的方法，其特征在于，所述根据所述含硫气体在所述取样温度和所述取样压力下的体积及所述元素硫的质量，计算得到所述含硫气体中的 元素硫的溶解度包括采用如下式(3)计算得到所述含硫气体中的元素硫的溶解度；
式(3)中，c——含硫气体中元素硫的溶解度；m——元素硫的质量；V 1'——含硫气体在取样温度和取样压力下的体积。 - 根据权利要求14所述的方法，其特征在于，该方法具体包括以下步骤：(1)采集含硫气藏中的含硫气体，测定采集所述含硫气体时的取样温度和取样压力；(2)将所述含硫气体转入配样器中，使所述配样器在预设温度及预设压力下摇摆预设时长，以防止含硫气体中的元素硫析出；(3)使步骤(2)中的含硫气体平衡降压至室压，之后流入吸附罐内，其中，所述吸附罐内盛放二硫化碳液体；(4)从所述吸附罐流出的气体通过气体流量计，所述气体流量计测定步骤(3)所得含硫气体在室温和所述室压下的体积；(5)将所述吸附罐内的二硫化碳液体收集并转移到收集罐内；加热所述收集罐以除去二硫化碳，冷却，测定所述收集罐内的元素硫的质量；(6)根据所述取样温度、所述取样压力、所述室温、所述室压、所述元素硫的质量及步骤(3)所得含硫气体在室温和所述室压下的体积，计算得到所述含硫气体中元素硫的溶解度。
- 根据权利要求19所述的方法，其特征在于，在步骤(5)之前，该方法还包括：采用二硫化碳液体清洗所述配样器与所述吸附罐之间的管线，再将清洗后的二硫化碳液体收集并转移到所述收集罐内。
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| CN118190700A (zh) * | 2024-05-17 | 2024-06-14 | 中国石油大学(华东) | 一种测量高温高压条件下气体溶解度的装置及使用方法 |
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