CN111693400A - Evaluation device of dynamic sulphur removal efficiency of sulphur removal agent - Google Patents

Evaluation device of dynamic sulphur removal efficiency of sulphur removal agent Download PDF

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Publication number
CN111693400A
CN111693400A CN202010434516.2A CN202010434516A CN111693400A CN 111693400 A CN111693400 A CN 111693400A CN 202010434516 A CN202010434516 A CN 202010434516A CN 111693400 A CN111693400 A CN 111693400A
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absorption
kettle
gas
pipeline
safety valve
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常振
铁磊磊
李翔
于萌
曾浩见
杜朝阳
董辉
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China Oilfield Services Ltd
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China Oilfield Services Ltd
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N7/00Analysing materials by measuring the pressure or volume of a gas or vapour
    • G01N7/02Analysing 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
    • G01N7/04Analysing 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

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Abstract

An evaluation device for the dynamic sulfur removal efficiency of a sulfur removal agent comprises: the device comprises a gas inlet unit, an absorption unit, a tail gas treatment unit and a data acquisition and treatment unit, wherein the absorption unit comprises gas buffering preheating equipment and gas absorption equipment, and the arrangement and connection relationship of each unit and equipment are as described in the specification. The evaluation device can obtain the dynamic desulphurization efficiency of the desulphurization agent, and provides data support for screening the desulphurization agent for oil field water treatment.

Description

Evaluation device of dynamic sulphur removal efficiency of sulphur removal agent
Technical Field
The application relates to an oil field desulphurization technology, in particular to an evaluation device for dynamic desulphurization efficiency of a desulphurization agent.
Background
At present, when the performance of the desulfurizing agent is evaluated, indoor evaluation can be carried out only by using a simple device constructed by a glass experimental instrument, the simple experimental device can only be used for measuring the static desulfurizing efficiency at normal temperature and normal pressure, and cannot simulate the process of coexistence and flowing of gas phase and liquid phase under the actual environment of an oil field, so that the dynamic desulfurizing (namely instantaneous desulfurizing) efficiency of the desulfurizing agent under the actual state of the oil field water treatment process cannot be evaluated. However, the water treatment process of offshore oil fields is very short, the desulfurization agent is required to rapidly remove sulfur instantly, and if the dynamic desulfurization efficiency of the desulfurization agent cannot be evaluated, the desulfurization agent with the optimal performance cannot be screened for the water treatment of oil fields, particularly offshore oil fields, so that the desulfurization result of the water treatment is influenced.
Disclosure of Invention
The application provides a device for evaluating desulfurizing agent sulphur removal efficiency can obtain the dynamic sulphur removal efficiency of desulfurizing agent through the device, provides data support for oil field water treatment screening desulfurizing agent.
Specifically, the application provides an evaluation device of dynamic sulphur removal efficiency of a sulphur removal agent, the device comprises:
an air intake unit comprising H with a flow meter2S gas cylinder, carrier gas cylinder with flow meter and corresponding pipeline, said H2The pipeline where the S gas cylinder is located and the pipeline where the carrier gas cylinder is located are converged into a converging pipeline through a three-way valve;
an absorption unit comprising:
the gas buffering preheating device comprises a closed buffering kettle and a first heater for heating the buffering kettle, an inlet pipeline of the buffering kettle is connected with the converging pipeline, a first temperature monitoring element is arranged in the buffering kettle, and the length of the part, located in the buffering kettle, of an outlet pipeline of the buffering kettle is larger than that of the part, located in the buffering kettle, of the inlet pipeline of the buffering kettle;
the gas absorption equipment comprises a closed absorption kettle and a second heater for heating the absorption kettle, the absorption kettle is arranged at the downstream of the buffer kettle, an inlet pipeline of the absorption kettle is connected with the confluence pipeline, the length of an outlet pipeline of the absorption kettle in the inner part of the absorption kettle is greater than that of an inlet pipeline of the absorption kettle in the inner part of the absorption kettle, and a sulfur removing agent and a second temperature monitoring element are arranged in the absorption kettle;
a tail gas treatment unit disposed downstream of the absorption kettle and connected with the converging pipeline, including for containing H2S, a tail gas absorption bottle of a gas absorbent, wherein the length of the part, positioned inside the tail gas absorption bottle, of an inlet pipeline of the tail gas absorption bottle is greater than the length of the part, positioned inside the tail gas absorption bottle, of an outlet pipeline of the tail gas absorption bottle;
the data acquisition and processing unit comprises a pressure sensor and data recording and processing equipment, one end of the pressure sensor is connected with the converging pipeline, the other end of the pressure sensor is connected with the data recording and processing equipment, and the first temperature monitoring element and the second temperature monitoring element are in signal connection with the data recording and processing equipment.
In the present application, "dynamic sulfur removal efficiency" refers to the absorption rate of a sulfur removal agent to a flowing hydrogen sulfide-containing gas of a certain amount and concentration in the flowing state.
In an embodiment of the present application, the gas absorption apparatus may further include a vacuum pump disposed between the absorption vessel and the off-gas treatment unit and connected to the confluence line.
In the embodiment of the application, the device for evaluating the dynamic sulfur removal efficiency of the sulfur removal agent can also comprise a safety valve,
when the gas absorption apparatus does not include a vacuum pump, the safety valve may be disposed in any one or two of the following manners: (1) a first safety valve is arranged on a converging pipeline between an inlet pipeline of the buffer kettle and the pressure sensor; (2) a second safety valve is arranged on a converging pipeline between the pressure sensor and the inlet pipeline of the absorption kettle;
when the gas absorption device comprises a vacuum pump, the safety valve is arranged in any one or more of the following three ways: (1) a first safety valve is arranged on a converging pipeline between an inlet pipeline of the buffer kettle and the pressure sensor; (2) a second safety valve is arranged on a converging pipeline between the pressure sensor and the inlet pipeline of the absorption kettle; (3) and a third safety valve is arranged on a converging pipeline between the inlet pipeline of the absorption kettle and the tail gas absorption bottle.
In an embodiment of the present application, the first safety valve and the second safety valve may be ball valves, and the third safety valve may be a needle valve.
In an embodiment of the present application, the tail gas treatment unit may further include a weighing device for weighing the tail gas absorption bottle, and the weighing device is disposed below the tail gas absorption bottle.
In embodiments of the present application, the off-gas treatment unit can include at least two off-gas absorber bottles in series.
In an embodiment of the present application, the second heater may have an agitation function configured to be able to agitate the sulfur removing agent in the sulfur removing agent container.
In an embodiment of the present application, the second heater may be a constant temperature magnetic stirrer, and the desulfurizing agent container is provided with a magneton therein.
In the embodiment of the application, the buffer kettle is made of 304 stainless steel or hastelloy gold, and the absorption kettle is made of 304 stainless steel or hastelloy gold;
in the embodiment of this application, can be provided with the desulfurizing agent container that is used for holding the desulfurizing agent in the absorption cauldron, the inner wall of desulfurizing agent container can be the polytetrafluoroethylene material, the second temperature monitoring component can set up in the desulfurizing agent container.
In an embodiment of the present application, the first heater may be a thermostatic heater, for example, a thermostatic water bath.
In the examples of the present application, said H2The flowmeter on the S gas cylinder can be a gas float flowmeter, and the flowmeter on the carrier gas cylinder can be a gas float flowmeter.
In an embodiment of the present application, the carrier gas in the carrier gas cylinder may be nitrogen.
In an embodiment of the present application, the three-way valve may be a three-way ball valve.
The evaluation device of the dynamic desulfurization efficiency of the desulfurizing agent is based on the constant volume principle, and according to the ideal gas equation PV ═ nR' T (in the formula, P represents the partial pressure in the absorption kettle, V represents the volume of the absorption kettle, and n represents H2The molar quantity of S gas, R' represents the parameters of a gas equation in a non-ideal state, and T represents the temperature in the absorption kettle). When the sulfur-removing agent absorbs H under the condition that V, R and T are constant and known2S gas, n is reduced, and P is also reduced, so that H can be determined by the change of the pressure P in the trapping device2The molar quantity n of S gas.
The evaluation device for the dynamic desulfurization efficiency of the desulfurizing agent can obtain the dynamic desulfurization efficiency of the desulfurizing agent, and provides data support for screening the desulfurizing agent with optimal performance for water treatment of oil fields, particularly offshore oil fields.
Additional features and advantages of the application will be set forth in the description which follows, and in part will be obvious from the description, or may be learned by the practice of the application. Other advantages of the present application may be realized and attained by the instrumentalities and combinations particularly pointed out in the specification and the drawings.
Drawings
The accompanying drawings are included to provide an understanding of the present disclosure and are incorporated in and constitute a part of this specification, illustrate embodiments of the disclosure and together with the examples serve to explain the principles of the disclosure and not to limit the disclosure.
FIG. 1 is a schematic view showing the structure of an apparatus for evaluating the dynamic sulfur removal efficiency of a sulfur remover according to an embodiment of the present invention.
The reference symbols in the drawings have the following meanings:
1-H2s, a gas cylinder; 2-a carrier gas cylinder; 3-a first three-way valve; 4-a buffer kettle; 5-a first heater; 6-a first temperature monitoring element; 7-absorption kettle; 8-a second heater; 9-a sulphur removal agent container; 10-a second temperature monitoring element; 11-magneton; 12-a vacuum pump; 13-a second three-way valve; 14-tail gas absorption bottle; 15-a pressure sensor; 16-a data recording and processing device; 17-a first safety valve; 18-a second safety valve; 19-third safety valve.
Detailed Description
To make the objects, technical solutions and advantages of the present application more apparent, embodiments of the present application will be described in detail below with reference to the accompanying drawings. It should be noted that the embodiments and features of the embodiments in the present application may be arbitrarily combined with each other without conflict.
The embodiment of the application provides an evaluation device of dynamic sulphur removal efficiency of a sulphur removal agent, as shown in fig. 1, the device comprises: the device comprises an air inlet unit, an absorption unit, a tail gas treatment unit and a data acquisition and treatment unit.
The air inlet unit comprises a H with a flow meter2S gas cylinder 1, carrier gas cylinder 2 with flowmeter and corresponding pipeline, mainly used for providing H with different concentrations and different pressures for the device of the embodiment of the application2S combined gas. Wherein H2S gas cylinder 1 provides H for dynamic sulphur removal efficiency test2S gas, carrier gas cylinder 2 provides dilution H2Carrier gas of S gas to provide different concentrations of H2S combined gas. The gas is output according to the designed flow through a flowmeter arranged on the gas cylinder, and H with different concentrations and different pressures can be compounded by adjusting the flowmeter2S combined gas. Said H2The flowmeter arranged on the S gas cylinder 1 can be a gas float flowmeter, and the flowmeter arranged on the carrier gas cylinder 2 is a gas float flowmeter. The carrier gas in the carrier gas cylinder 2 may be nitrogen. Said H2And the pipeline where the S gas cylinder 1 is located and the pipeline where the carrier gas cylinder 2 is located are converged into a converging pipeline through a first three-way valve 3.
The absorption unit comprises a gas buffer preheating device and a gas absorption device.
The gas buffer preheating device is mainly used for H coming from the gas inlet unit2The S combined gas is preheated and buffered, and H can be avoided by preheating2And the S combined gas enters the gas absorption equipment and then is subjected to large-amplitude temperature adjustment, and the designed temperature can be reached only by carrying out small adjustment, so that accurate temperature control is realized. The gas buffering preheating device comprises a closed buffering kettle 4 and a first heater 5 for heating the buffering kettle. The inner surface and the outer surface of the buffer kettle 4 can be coated with polytetrafluoroethylene anticorrosive coatings to prevent H2S, corrosion of the combined gas; the kettle cover and the kettle body are hermetically connected through the flange screws, and the inner surface of the kettle cover can be coated with the silicone rubber layer, so that the sealing performance of the kettle body is ensured. An inlet line of the buffer tank 4 is connected to the confluence line, and a first temperature monitoring element 6, which may be a thermocouple or the like, is disposed inside the buffer tank 4. The temperature inside the buffer tank 4 is monitored by the first temperature monitoring element 6, and the set temperature of the first heater 5 is adjusted in accordance with the temperature inside the buffer tank 4 monitored by the first temperature monitoring element 6. The first heater 5 may be a constant temperature heater, for example, a constant temperature water bath, and the constant temperature heater may be implemented for H in the buffer tank 42And (4) accurately heating and preheating the S combined gas. Because the buffer tank 4 is heated under pressure, the buffer tank 4 is required to have certain rigidity, and the material of the buffer tank 4 may be stainless steel, for example, 304 stainless steel, or hastelloy gold. The outlet pipeline of the buffer kettle 4 is in the length of the inner part of the buffer kettle 4 is larger than the inlet pipeline of the buffer kettle 4 is in the length of the inner part of the buffer kettle 4, so that gas backflow can be prevented, and the experimental gas is ensured to be closer to the site environment and the safety of the whole device.
The gas absorption device comprises a closed absorption kettle 7 and a second heater 8 for heating the absorption kettle. The absorption kettle 7 is arranged at the downstream of the buffer kettle 4, the inlet pipeline of the absorption kettle 7 is connected with the confluence pipeline, the length of the part of the outlet pipeline of the absorption kettle 7, which is positioned in the absorption kettle 7, is larger than that of the inlet pipeline of the absorption kettle 7The length of the inner part of the absorption kettle 7 can prevent gas backflow and suck back. A desulfurizing agent container 9 for containing a desulfurizing agent is arranged in the absorption kettle 7, and a second temperature monitoring element 10, such as a thermocouple and the like, is arranged in the desulfurizing agent container 9. In other embodiments, the sulfur remover container 9 may not be provided, the sulfur remover may be directly placed in the absorption vessel 7, and the second temperature monitoring element 10 may be provided in the absorption vessel 7. The material of the absorption kettle 7 can be 304 stainless steel or hastelloy. The material of the inner wall of the desulfurizing agent container 9 can be polytetrafluoroethylene and the like. The second heater 8 may have a stirring function and is configured to stir the desulfurizing agent in the desulfurizing agent container 9 to promote the H2And fully contacting the S combined gas with a sulfur removal agent. The second heater 8 can be a constant-temperature magnetic stirrer, and a magneton 11 is arranged in the desulfurizing agent container 9. By heating the absorption kettle 7 under pressure, the actual temperature and pressure environment of an oil field site can be simulated, and reliable data support is provided for screening the desulfurizing agent for oil field water treatment.
As shown in fig. 1, the gas absorption apparatus may further include a vacuum pump 12, and the vacuum pump 12 is disposed between the absorption vessel 7 and the off-gas treatment unit and connected to the confluence line. The vacuum pump 12 can provide a slight negative pressure to prevent gas leakage in the pipeline.
The off-gas treatment unit is disposed downstream of the absorption vessel 7 and connected to the confluence line, and the confluence line, the line in which the vacuum pump 7 is located, and the line in which the off-gas treatment unit is located are connected by a second three-way valve 13 (e.g., a three-way ball valve). The tail gas treatment unit comprises a tank for containing H2S gas absorbent tail gas absorption bottle 14, the length of the inlet pipeline of the tail gas absorption bottle 14 in the inner part of the tail gas absorption bottle 14 is greater than the length of the outlet pipeline of the tail gas absorption bottle 14 in the inner part of the tail gas absorption bottle 14. The off-gas treatment unit can include at least two off-gas absorber bottles 14 in series. In the device shown in fig. 1, two tail gas absorption bottles 14 are arranged in series, and in other embodiments, more tail gas absorption bottles 14 can be arranged in series to avoidH-free2And S gas is discharged from the outlet. The tail gas absorption bottle can be made of glass, stainless steel and other materials, and can be made of 316 steel, for example. H contained in tail gas absorption bottle 142The S gas absorbent may be a sodium hydroxide solution, a potassium hydroxide solution, ammonia water, etc., for example, a 10 wt% sodium hydroxide solution. The tail gas absorption bottle 14 can be provided with a weighing device for weighing the tail gas absorption bottle 14, the mass before and after tail gas absorption can be weighed, and the static sulfur capacity and the average absorption efficiency (through H) of the sulfur removal agent in a period of time can be calculated through a differential method2The flowmeter of the S gas cylinder and the flowmeter of the carrier gas cylinder can obtain H2The total amount of the S combined gas is subtracted by the weight gain of the tail gas absorption bottle 14 to calculate the H absorbed by the desulfurizing agent2S amount, and then the static sulfur capacity and average absorption efficiency of the sulfur removal agent).
The data acquisition and processing unit comprises a pressure sensor 15, one end of which is connected to the converging line and the other end of which is connected to the data recording and processing device 16, and a data recording and processing device 16. Sulfur removal agent absorbs H2After S, the instantaneous partial pressure in the absorption kettle is reduced, the pressure signal is transmitted to the pressure sensor 15, the pressure sensor 15 converts the pressure signal into an electromagnetic signal and transmits the electromagnetic signal to the data recording and processing device 16, and the instantaneous pressure change and the pressure change value of each time are recorded. The data recording and processing device 16 may include a paperless recorder and a computer, and the data recorded by the paperless recorder may be processed by the computer to derive the dynamic sulfur removal (i.e., instantaneous sulfur removal) efficiency of the sulfur removal agent. The first temperature monitoring element 6 and the second temperature monitoring element 10 are in signal connection with the data recording and processing device 16, and the first heater 5 and the second heater 8 are controlled to heat and stop heating through the data recording and processing device 16.
The device of the embodiments of the present application may also include a safety valve. For example, a first safety valve 17 may be provided on a junction line between the inlet line of the buffer tank 4 and the pressure sensor 15, a second safety valve 18 may be provided on a junction line between the pressure sensor 17 and the inlet line of the absorption tank 7, and when the gas absorption device includes the vacuum pump 12, a third safety valve 19 may be further provided on a junction line between the inlet line of the absorption tank 7 and the off-gas absorption bottle 14. The first safety valve 17 and the second safety valve 18 may be both ball valves, and the third safety valve may be a needle valve.
In the description of the embodiments of the present application, it should be noted that the terms "one end", "the other end", and the like indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, which are only used for convenience in describing the present application and simplifying the description, but do not indicate or imply that the structures referred to have specific orientations, are configured and operated in specific orientations, and thus, should not be construed as limiting the present application.
In the description of the embodiments of the present application, unless explicitly stated or limited otherwise, the terms "connected" and "disposed" are to be understood broadly, e.g., they may be fixedly connected, detachably connected, or integrally connected; the terms "connected" and "disposed" may be directly connected or indirectly connected through intervening media, and may be internal to both elements. The specific meaning of the above terms in the present application can be understood in a specific case by those of ordinary skill in the art.
Although the embodiments disclosed in the present application are described above, the descriptions are only for the convenience of understanding the present application, and are not intended to limit the present application. It will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the disclosure as defined by the appended claims.

Claims (10)

1. An evaluation device for the dynamic sulfur removal efficiency of a sulfur removal agent, characterized by comprising:
an air intake unit comprising H with a flow meter2S gas cylinder with flowmeterCarrier gas cylinder and corresponding line, said H2The pipeline where the S gas cylinder is located and the pipeline where the carrier gas cylinder is located are converged into a converging pipeline through a three-way valve;
an absorption unit comprising:
the gas buffering preheating device comprises a closed buffering kettle and a first heater for heating the buffering kettle, an inlet pipeline of the buffering kettle is connected with the converging pipeline, a first temperature monitoring element is arranged in the buffering kettle, and the length of the part, located in the buffering kettle, of an outlet pipeline of the buffering kettle is larger than that of the part, located in the buffering kettle, of the inlet pipeline of the buffering kettle;
the gas absorption equipment comprises a closed absorption kettle and a second heater for heating the absorption kettle, the absorption kettle is arranged at the downstream of the buffer kettle, an inlet pipeline of the absorption kettle is connected with the confluence pipeline, the length of an outlet pipeline of the absorption kettle in the inner part of the absorption kettle is greater than that of an inlet pipeline of the absorption kettle in the inner part of the absorption kettle, and a sulfur removing agent and a second temperature monitoring element are arranged in the absorption kettle;
a tail gas treatment unit disposed downstream of the absorption kettle and connected with the converging pipeline, including for containing H2S, a tail gas absorption bottle of a gas absorbent, wherein the length of the part, positioned inside the tail gas absorption bottle, of an inlet pipeline of the tail gas absorption bottle is greater than the length of the part, positioned inside the tail gas absorption bottle, of an outlet pipeline of the tail gas absorption bottle;
the data acquisition and processing unit comprises a pressure sensor and data recording and processing equipment, one end of the pressure sensor is connected with the converging pipeline, the other end of the pressure sensor is connected with the data recording and processing equipment, and the first temperature monitoring element and the second temperature monitoring element are in signal connection with the data recording and processing equipment.
2. The apparatus of claim 1, wherein the gas absorption device further comprises a vacuum pump disposed between the absorption vessel and the off-gas treatment unit and connected to the junction line.
3. The device of claim 1 or 2, further comprising a safety valve,
when the gas absorption apparatus does not include a vacuum pump, the safety valve may be disposed in any one or two of the following manners: (1) a first safety valve is arranged on a converging pipeline between an inlet pipeline of the buffer kettle and the pressure sensor; (2) a second safety valve is arranged on a converging pipeline between the pressure sensor and the inlet pipeline of the absorption kettle;
when the gas absorption device comprises a vacuum pump, the safety valve is arranged in any one or more of the following three ways: (1) a first safety valve is arranged on a converging pipeline between an inlet pipeline of the buffer kettle and the pressure sensor; (2) a second safety valve is arranged on a converging pipeline between the pressure sensor and the inlet pipeline of the absorption kettle; (3) a third safety valve is arranged on a converging pipeline between the inlet pipeline of the absorption kettle and the tail gas absorption bottle;
optionally, the first safety valve and the second safety valve are both ball valves, and the third safety valve is a needle valve.
4. The apparatus according to claim 1 or 2, wherein the tail gas treatment unit further comprises a weighing device for weighing the tail gas absorption bottle, the weighing device being disposed below the tail gas absorption bottle;
optionally, the off-gas treatment unit comprises at least two off-gas absorber bottles in series.
5. The apparatus according to claim 1 or 2, wherein the second heater has an agitation function configured to be capable of agitating the desulfurizing agent in the desulfurizing agent container;
optionally, the second heater is a constant temperature magnetic stirrer, and the inside of the sulfur remover container is provided with magnetons.
6. The device of claim 1 or 2, wherein the buffer tank is made of 304 stainless steel or Hastelloy, and the absorption tank is made of 304 stainless steel or Hastelloy;
optionally, a desulfurizing agent container for containing a desulfurizing agent is arranged in the absorption kettle, the inner wall of the desulfurizing agent container is made of polytetrafluoroethylene, and the second temperature monitoring element is arranged in the desulfurizing agent container.
7. The apparatus of claim 1 or 2, wherein the first heater is a thermostatic heater, optionally a thermostatic water bath.
8. The apparatus of claim 1 or 2, wherein the H is2The gas cylinder S is provided with a flowmeter which is a gas float flowmeter, and the carrier gas cylinder S is provided with a flowmeter which is a gas float flowmeter.
9. The apparatus of claim 1 or 2, wherein the carrier gas in the carrier gas cylinder is nitrogen.
10. The apparatus of claim 1 or 2, wherein the three-way valve is a three-way ball valve.
CN202010434516.2A 2020-05-21 2020-05-21 Evaluation device of dynamic sulphur removal efficiency of sulphur removal agent Pending CN111693400A (en)

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周杨 等: "钻井液中硫化氢污染特点及高效除硫剂性能评价", 《石油化工应用》 *
李晓艳 等: "克浅井区稠油热采套管气除H_2S研究与应用", 《新疆石油科技》 *
李树刚 等: "钻井液除硫剂吸收硫化氢动态评价方法研究", 《石油与天然气化工》 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112782158A (en) * 2020-12-28 2021-05-11 杭州电子科技大学 Monitoring system for crude copper desulfurization
CN112782158B (en) * 2020-12-28 2023-09-08 杭州电子科技大学 Monitoring system for blister copper desulfurization

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