Device and method for detecting desulfurization rate of a liquid desulfurizer product under high-temperature conditions

Abstract

The present invention relates to a detection device for the desulfurization rate of a liquid desulfurizer product under high-temperature conditions, comprising a reaction vessel, a sealing upper cover, a sealing bottle stopper, a conduit, and a sealing clip; the sealing upper cover is located at the upper opening of the reaction vessel and is used to form a sealed reaction environment for the reaction vessel; the sealing upper cover is provided with a through hole for the conduit to pass through and an opening for placing the sealing bottle stopper; the conduit passes through the through hole and extends into the reaction vessel to a position in the middle of the reaction vessel, and a sealed condition is maintained between the conduit and the through hole; the sealing clip is clamped at one end of the conduit exposed outside the reaction vessel and is used to seal the part of the conduit communicating with the outside. The structure of the present invention is simple, the test process is fully sealed, and the detection result has high accuracy.

Description

Technical Field

[0001] The present invention relates to the field of oil fields, and particularly to a device and a method for detecting the desulfurization rate of a liquid desulfurizer product under high-temperature conditions. Background Art

[0002] Hydrogen sulfide, CO2, and organic sulfides contained in natural gas, coal gas, biogas, industrial waste gas, and refinery gas can generally be collectively referred to as acidic components. The organic sulfides mainly include carbonyl sulfide, carbon disulfide, and sulfides such as mercaptans and thioethers with different carbon numbers. A large number of sulfide components present in oil and gas not only cause corrosion of equipment and pipelines during extraction, treatment, storage, and transportation, but also bring environmental pollution and seriously endanger the health of users when used as fuel; when used as a chemical raw material, it will cause poisoning of downstream catalysts. Since organic sulfur compounds have an impact on environmental protection, equipment corrosion, and human health, strict regulations have been made on the content (or total sulfur) of organic sulfur in commercial gas in various countries. Therefore, the removal of organic sulfur from natural gas and refinery gas has always been a research topic and a difficult problem that has received much attention in the purification process. Whether oil and gas are used for civilian or industrial purposes, the acidic components in them must be effectively removed before being output as commercial gas to meet the index requirements of pipeline transportation or commercial gas. The purpose of removing acidic components in natural gas is to remove the acidic components in oil and gas to the required index according to different uses.

[0003] A desulfurizer generally refers to a reagent for removing free sulfur or sulfur compounds in fuels, raw materials, or other materials; in the control and treatment of pollutants, it mainly refers to a reagent that can remove sulfur oxides (including SO2 and SO3) in waste gas. Various alkaline compounds can be used as desulfurizers.

[0004] For the desulfurizer for removing sulfur dioxide in flue gas, the most commonly used ones are inexpensive lime, limestone, and alkaline solutions prepared with lime-based reagents. The desulfurizer can absorb most of the sulfur dioxide in the flue gas and fix it in the fuel slag. Chemical plants, smelters, etc. often use solutions such as sodium carbonate and basic aluminum sulfate as desulfurizers to treat tail gas containing sulfur dioxide, and can desorb and recycle them.

[0005] This mixed-solution desulfurizer has surface activity and catalytic oxidation properties, which can promote the direct reaction of SO2, accelerate the dissolution of CaCO3, promote the rapid oxidation of CaSO3 into CaSO4, strengthen the precipitation of CaSO4, reduce the liquid-gas ratio, decrease the calcium-sulfur ratio, and reduce the evaporation of water. When the SO2 concentration at the flue gas inlet increases and is higher than the design value, and when a larger Ca / S ratio is required due to the decrease in the pH value in the reaction pool of the absorption tower, without the need to expand the volume of the reaction pool in the absorption tower, CaCO3 can dissolve quickly, increase the calcium ion concentration, maintain the pH value of the slurry within the normal range, and have a certain buffering effect on the pH value. Prolonging the operation time of the slurry in the working section and reducing the number of slurry preparation times can significantly reduce equipment scaling, make the scale layer thinner, and the scale layer is easily shed after flushing with water during shutdown. It has a dispersing and active effect on the scaling of the desulfurization system, reduces the accumulation of scale, decreases the chloride ion content in the slurry, and reduces the corrosion and scaling rates of various materials in the desulfurization equipment to varying degrees. Among them, the carbon steel reduction is the most significant, and the corrosion and scaling rates can be reduced by 74% and 79% respectively, and polyvinyl chloride can be reduced by 48% and 55%. The addition of the desulfurizer can play a role in scale inhibition, corrosion prevention, and corrosion inhibition, reduce the blockage, scaling, corrosion, and wear of the desulfurization nozzles, reduce the scaling, corrosion, and wear of the slurry circulation pump and its impeller, and reduce the maintenance and replacement of spare parts in the desulfurization system. It broadens the selection range of desulfurization materials and improves the reliability of the system. Under different operating conditions, it can reduce and stop the slurry circulation pump and the oxidation fan, improve the desulfurization efficiency, reduce the operating cost, adapt to the change of sulfur content in coal, and is suitable for high-sulfur coal. In the application of flue gas desulfurization, it has broad market promotion advantages and can generate considerable economic and social benefits.

[0006] CN204034544U discloses a flue gas denitrification, desulfurization, and dust recovery and separation device, including a denitrification separator and a desulfurization separator in a double-body series connection; the desulfurization and dust separator is also an integrated series connection device. The top flue gas outlet of the denitrification separator is connected to the lower flue gas inlet of the desulfurization separator. After desulfurization, the dust naturally precipitates and is removed under gravity. The flue gas denitrification, desulfurization, and dust recovery and separation device proposed by the present utility model adopts the cold-state selection method. For denitrification, the temperature range for denitrification is (120 - 170°C). The copper-ammonia complex solution and acidic components such as H2S in the coal gas enter the liquid phase from the gas phase and react with ammonia to be converted into acidic ammonium salts such as ammonium hydrosulfide, and then are converted into elemental sulfur under the oxidation of air. It selectively reduces NOx in the flue gas to N2 and water to reduce NO x emission technology, which has high denitrification efficiency. Generally, the NO x removal rate can reach more than 90%; after the flue gas is denitrified, it enters the desulfurization system. The project uses sodium hydroxide (or lime emulsion) and adopts a one-furnace-one-tower desulfurization device, and the desulfurization rate is not less than 91.2%.

[0007] CN103789003A discloses a method for measuring the reactivity of a desulfurization adsorbent. In this method, it is carried out in an adsorption desulfurization device, which includes an adsorption desulfurization reaction system, a sampling system, and a detection and analysis system connected in sequence along the material flow direction. In the method of the present invention, by arranging the sampling system and the detection and analysis system after the adsorption desulfurization reaction system in the adsorption desulfurization device, the method of the present invention can effectively and real-time analyze the samples obtained at different time periods, so as to better and more accurately measure the performance of the adsorbent.

[0008] However, in the prior art, there is no device for detecting the desulfurization rate of liquid desulfurizing agents. There are many types of liquid desulfurizing agent products, but currently, there is no unified detection and evaluation method for liquid desulfurizing agents. Due to the high toxicity of hydrogen sulfide, higher requirements are put forward for the safety of laboratory evaluations. Developing a desulfurizing agent evaluation method with strong operability and high safety has become an urgent research work to be carried out currently. Summary of the Invention

[0009] Therefore, the present invention provides a device for detecting the desulfurization rate of a liquid desulfurizing agent product under high-temperature conditions, including a reaction container, a sealing upper cover, a sealing bottle stopper, a conduit, and a sealing clip; the sealing upper cover is located at the upper opening of the reaction container to form a sealed reaction environment for the reaction container; a through hole for the conduit to pass through and an opening for placing the sealing bottle stopper are provided on the sealing upper cover; the conduit passes through the through hole and extends into the reaction container to a position in the middle of the reaction container, and a sealed condition is maintained between the conduit and the through hole; the sealing clip is clamped at one end of the conduit exposed outside the reaction container to seal the part of the conduit communicating with the outside.

[0010] Further, the reaction container is a wide-mouth reaction bottle.

[0011] Further, the sealing bottle stopper is a rubber bottle stopper.

[0012] Further, the conduit is a rubber conduit.

[0013] Further, the sealing clip is a conduit clip.

[0014] The working principle of the device for detecting the desulfurization rate of a liquid desulfurizing agent product under high-temperature conditions according to the present invention is as follows: In a sealed reaction container, a trace amount of hydrogen sulfide gas is formed with a reagent (divided into a blank sample reaction container and a test sample reaction container), and then a test amount of liquid desulfurizing agent is added. After the reaction test time, the content of hydrogen sulfide gas in the reaction containers with the liquid desulfurizing agent added (test sample reaction container) and without the liquid desulfurizing agent added (blank sample reaction container) is respectively measured, and the desulfurization rate of the liquid desulfurizing agent is calculated through a formula.

[0015] The present invention further provides a method for detecting the desulfurization rate using the aforementioned desulfurization rate detection device, including the following steps:

[0016] Step (1), preparation of the desulfurization detection device: Install the desulfurization detection device as required. The upper cover, bottle stopper, conduit, and sealing clip are all installed as required to form a sealed environment inside the reaction vessel. After detecting the airtightness of the desulfurization detection device, it is ready for use;

[0017] Step (2), preparation of chemical reagents: Weigh Na2S·9H2O, add deionized water, and prepare a sodium sulfide solution with a mass concentration of 0.1 - 10% for standby; Weigh concentrated sulfuric acid with a concentration of 98%, add deionized water, and prepare a dilute sulfuric acid solution with a mass concentration of 0.5 - 5% for standby;

[0018] Step (3), preparation of a blank sample reaction vessel: Add 2.0 - 10 g of the sodium sulfide solution in step (2) to the reaction vessel, then add 80 - 200 g of deionized water. After obtaining a homogeneous solution, add 0.1 - 5 ml of the dilute sulfuric acid solution, and then quickly cover the upper sealing cover. Keep the reaction vessel at a constant temperature, shake well and react to obtain a blank sample reaction vessel;

[0019] Step (3), preparation of a test sample reaction vessel: Under exactly the same conditions as in step (3), prepare a test sample reaction vessel. After shaking well and reacting, use a syringe to inject a test amount of liquid desulfurizer into the test sample reaction vessel through the sealing plug, shake well and carry out the desulfurization reaction to obtain a test sample reaction vessel;

[0020] Step (4), detection of hydrogen sulfide gas concentration: After the reactions in the blank sample reaction vessel and the test sample reaction vessel are sufficient, use a hydrogen sulfide detection tube to test the hydrogen sulfide gas concentration in the blank sample reaction vessel to obtain the hydrogen sulfide concentration M0 in the blank sample reaction vessel; Use a hydrogen sulfide detection tube to test the hydrogen sulfide gas concentration in the test sample reaction vessel to obtain the hydrogen sulfide concentration M1 in the test sample reaction vessel;

[0021] Step (5), calculation of the desulfurization rate of the test sample liquid desulfurizer:

[0022]

[0023] In the formula, X is the desulfurization rate, M0 is the hydrogen sulfide concentration in the blank sample reaction vessel obtained in step (4), in mg / L, and M1 is the hydrogen sulfide concentration in the test sample reaction vessel obtained in step (4), in mg / L.

[0024] Further, in the step (2), 1.0 g of Na2S·9H2O is weighed, added with deionized water, and prepared into a sodium sulfide solution with a mass concentration of 1% for standby.

[0025] Further, in the step (2), 1.53 g of concentrated sulfuric acid with a concentration of 98% is weighed, added with 98.47 g of deionized water, and prepared into a dilute sulfuric acid solution with a mass concentration of 1.5% for standby.

[0026] Further, in the step (3), 6 g of the sodium sulfide solution prepared in the step (2) is added to a 500 ml reaction vessel, then 100 g of deionized water is added. After obtaining a homogeneous solution, 0.64 ml of the dilute sulfuric acid solution with a mass concentration of 1.5% is added.

[0027] Further, in the step (3), the sealing upper cover is quickly covered, and the reaction vessel is kept at a constant temperature of 50 °C.

[0028] Further, in the step (4), the liquid desulfurizer added to the test sample reaction vessel is a triazine-based liquid desulfurizer.

[0029] Further, in the step (4), the addition amount of the liquid desulfurizer is 100 μl.

[0030] Further, to maintain the accuracy of the test, it is preferred that the hydrogen sulfide concentration in the blank sample reaction vessel and the test sample reaction vessel without adding the liquid desulfurizer is above 600 mg / L.

[0031] Further, after adding the liquid desulfurizer in the step (4), the reaction time is 30 min, 45 min or 90 min.

[0032] The beneficial effects of the present invention are as follows: The present invention provides a test device and a test method for the desulfurization rate of a liquid desulfurizer, with a simple operation process and no generation of a large amount of pollutants. The entire experimental process of the present invention is kept in a closed state to minimize the harm of hydrogen sulfide to experimental personnel. The present invention mainly tests the absorption rate of hydrogen sulfide gas, which is more in line with the actual situation of removing hydrogen sulfide at the wellhead of an oil well on site, and the experimental results have great guiding significance for the site. Description of the Drawings

[0033] In the drawings, unless otherwise specified, the same reference numerals throughout the multiple drawings denote the same or similar components or elements. The drawings schematically illustrate various embodiments discussed in the present application by way of example and not limitation. These drawings are not necessarily drawn to scale.

[0034] Figure 1 A preferred embodiment of the detection device of the present invention.

[0035] 1 Reaction wide-mouth bottle; 2 Sealing upper cover; 3 Sealing plug; 4 Conduit; 5 Sealing clip. Detailed implementation manners

[0036] In the following text, only some exemplary embodiments are simply described. As those skilled in the art can recognize, the described embodiments can be modified in various different ways without departing from the spirit or scope of the present invention. Therefore, the drawings and the description are considered to be exemplary in nature rather than restrictive.

[0037] Before discussing the exemplary embodiments in more detail, it should be mentioned that some exemplary embodiments are described as processes or methods depicted as flowcharts. Although the flowcharts describe the operations as sequential processes, many of the operations can be implemented in parallel, concurrently, or simultaneously. In addition, the order of the operations can be rearranged. The process can be terminated when its operations are completed, but it can also have additional steps not included in the drawings. The process can correspond to a method, function, procedure, subroutine, subprogram, etc.

[0038] Figure 1 For a preferred implementation manner of the present invention, the desulfurization rate detection device includes a reaction wide-mouth bottle 1, a sealing upper cover 2, a sealing bottle plug 3, a conduit 4, and a sealing clip 5; the sealing upper cover 2 is located at the upper opening of the reaction wide-mouth bottle 1 and is used to form a sealed reaction environment for the reaction wide-mouth bottle 1; the sealing upper cover 2 is provided with a through hole for the conduit 4 to pass through and an opening for placing the sealing bottle plug 3; the conduit 4 passes through the through hole and extends into the reaction wide-mouth bottle 1 to a position in the middle of the reaction wide-mouth bottle 1, and a sealing condition is maintained between the conduit 4 and the through hole; the sealing clip 5 is clamped at one end of the conduit 4 exposed outside the reaction wide-mouth bottle and is used to seal the part of the conduit 4 communicating with the outside.

[0039] The preferred detection method implementation manner of the present invention is as follows:

[0040] Example 1

[0041] A method for detecting the desulfurization rate using the aforementioned desulfurization rate detection device includes the following steps:

[0042] Step (1), preparation of the desulfurization detection device: Install the desulfurization detection device as required, install the sealing upper cover, the sealing bottle plug, the conduit, and the sealing clip as required, form a sealed environment inside the reaction container, and after detecting the airtightness of the desulfurization detection device, set it aside for use;

[0043] Step (2), preparation of chemical reagents: Weigh 1.0 g of Na2S·9H2O, add 99.0 g of deionized water to prepare a sodium sulfide solution with a mass concentration of 1% for standby; weigh concentrated sulfuric acid with a concentration of 98%, add 500 ml of deionized water to prepare a dilute sulfuric acid solution with a mass concentration of 1.5% for standby;

[0044] Step (3), preparation of a blank sample reaction container: Take 6.0 g of the sodium sulfide solution from step (2) and add it to the reaction container, then add 100 g of deionized water. After obtaining a homogeneous solution, add 0.64 ml of the dilute sulfuric acid solution, and then quickly cover the sealing lid. Keep the reaction container at a constant temperature of 50 °C, shake well and react to obtain a blank sample reaction container;

[0045] Step (3), preparation of a test sample reaction container: Under exactly the same conditions as in step (3), prepare a test sample reaction container. After shaking well and reacting, use a syringe to inject 100 μL of a liquid desulfurizer (preferably a triazine-based liquid desulfurizer) into the test sample reaction container through the sealing plug, shake well and carry out a desulfurization reaction at a constant temperature of 50 °C for 30 min to obtain a test sample reaction container;

[0046] Step (4), detection of hydrogen sulfide gas concentration: After the reactions in the blank sample reaction container and the test sample reaction container are sufficient, use a hydrogen sulfide detection tube to test the hydrogen sulfide gas concentration in the blank sample reaction container to obtain the hydrogen sulfide concentration M0 in the blank sample reaction container; use a hydrogen sulfide detection tube to test the hydrogen sulfide gas concentration in the test sample reaction container to obtain the hydrogen sulfide concentration M1 in the test sample reaction container;

[0047] Step (5), calculation of the desulfurization rate of the test sample liquid desulfurizer:

[0048]

[0049] In the formula, X is the desulfurization rate, M0 is the hydrogen sulfide concentration in the blank sample reaction container obtained in step (4), in mg / L, and M1 is the hydrogen sulfide concentration in the test sample reaction container obtained in step (4), in mg / L. The calculated desulfurization rate in the test sample reactor is 98%.

[0050] Example 2

[0051] A method for detecting the desulfurization rate using the aforementioned desulfurization rate detection device, comprising the following steps:

[0052] Step (1), preparation of the desulfurization detection device: Install the desulfurization detection device as required. The upper sealing cover, sealing bottle stopper, conduit, and sealing clip are all installed as required to form a sealed environment inside the reaction vessel. After detecting the airtightness of the desulfurization detection device, it is ready for use;

[0053] Step (2), preparation of chemical reagents: Weigh 2.0 g of Na2S·9H2O and add 98.0 g of deionized water to prepare a sodium sulfide solution with a mass concentration of 2% for standby; Weigh concentrated sulfuric acid with a concentration of 98% and add 500 ml of deionized water to prepare a dilute sulfuric acid solution with a mass concentration of 1.5% for standby;

[0054] Step (3), preparation of a blank sample reaction vessel: Take 4.0 g of the sodium sulfide solution from step (2) and add it to the reaction vessel, then add 100 g of deionized water. After obtaining a homogeneous solution, add 1.3 ml of the dilute sulfuric acid solution, and then quickly cover the upper sealing cover. Keep the reaction vessel at a constant temperature of 50 °C, shake well and react to obtain a blank sample reaction vessel;

[0055] Step (3), preparation of a test sample reaction vessel: Under exactly the same conditions as in step (3), prepare a test sample reaction vessel. After shaking well and reacting, use a syringe to inject 100 μL of liquid desulfurizer (preferably a triazine-based liquid desulfurizer) into the test sample reaction vessel through the sealing plug, shake well and keep it at a constant temperature of 50 °C for 30 min for desulfurization reaction to obtain a test sample reaction vessel;

[0056] Step (4), detection of hydrogen sulfide gas concentration: After the reactions in the blank sample reaction vessel and the test sample reaction vessel are completed, use a hydrogen sulfide detection tube to test the hydrogen sulfide gas concentration in the blank sample reaction vessel to obtain the hydrogen sulfide concentration M0 in the blank sample reaction vessel; Use a hydrogen sulfide detection tube to test the hydrogen sulfide gas concentration in the test sample reaction vessel to obtain the hydrogen sulfide concentration M1 in the test sample reaction vessel;

[0057] Step (5), calculation of the desulfurization rate of the test sample liquid desulfurizer:

[0058]

[0059] In the formula, X is the desulfurization rate, M0 is the hydrogen sulfide concentration in the blank sample reaction vessel obtained in step (4), in mg / L, and M1 is the hydrogen sulfide concentration in the test sample reaction vessel obtained in step (4), in mg / L. The desulfurization rate in the test sample reactor is 97.6%.

[0060] Example 3

[0061] A method for detecting the desulfurization rate using the aforementioned desulfurization rate detection device, comprising the following steps:

[0062] Step (1), preparation of the desulfurization detection device: Install the desulfurization detection device as required. The upper sealing cover, sealing bottle stopper, conduit, and sealing clip are all installed as required to form a sealed environment inside the reaction vessel. After detecting the airtightness of the desulfurization detection device, set it aside for use;

[0063] Step (2), preparation of chemical reagents: Weigh 3.5 g of Na2S·9H2O and add 96.5 g of deionized water to prepare a sodium sulfide solution with a mass concentration of 3.5% for standby; Weigh concentrated sulfuric acid with a concentration of 98% and add 500 ml of deionized water to prepare a dilute sulfuric acid solution with a mass concentration of 1.5% for standby;

[0064] Step (3), preparation of a blank sample reaction vessel: Take 8.0 g of the sodium sulfide solution from step (2) and add it to the reaction vessel, then add 100 g of deionized water. After obtaining a homogeneous solution, add 3.0 ml of the dilute sulfuric acid solution, and then quickly cover the upper sealing cover. Keep the reaction vessel at a constant temperature of 50 °C, shake well and react to obtain a blank sample reaction vessel;

[0065] Step (3), preparation of a test sample reaction vessel: Under exactly the same conditions as in step (3), prepare a test sample reaction vessel. After shaking well and reacting, use a syringe to inject 100 μL of liquid desulfurizer (preferably a triazine-based liquid desulfurizer) into the test sample reaction vessel through the sealing plug, shake well, and keep it at a constant temperature of 50 °C for 30 min for desulfurization reaction to obtain a test sample reaction vessel;

[0066] Step (4), detection of hydrogen sulfide gas concentration: After the reactions in the blank sample reaction vessel and the test sample reaction vessel are sufficient, use a hydrogen sulfide detection tube to test the hydrogen sulfide gas concentration in the blank sample reaction vessel to obtain the hydrogen sulfide concentration M0 in the blank sample reaction vessel; Use a hydrogen sulfide detection tube to test the hydrogen sulfide gas concentration in the test sample reaction vessel to obtain the hydrogen sulfide concentration M1 in the test sample reaction vessel;

[0067] Step (5), calculation of the desulfurization rate of the test sample liquid desulfurizer:

[0068]

[0069] In the formula, X is the desulfurization rate, M0 is the hydrogen sulfide concentration in the blank sample reaction vessel obtained in step (4), in mg / L, and M1 is the hydrogen sulfide concentration in the test sample reaction vessel obtained in step (4), in mg / L. The desulfurization rate in the test sample reactor is 98%.

[0070] Example 4

[0071] A method for detecting the desulfurization rate using the aforementioned desulfurization rate detection device, comprising the following steps:

[0072] Step (1), preparation of the desulfurization detection device: Install the desulfurization detection device as required. The upper sealing cover, sealing bottle stopper, conduit, and sealing clip are all installed as required, so as to form a sealed environment inside the reaction vessel. After detecting the airtightness of the desulfurization detection device, set it aside for use;

[0073] Step (2), preparation of chemical reagents: Weigh 1.7 g of Na2S·9H2O, add 98.3 g of deionized water, and prepare a sodium sulfide solution with a mass concentration of 1% for standby; Weigh concentrated sulfuric acid with a concentration of 98%, add 500 ml of deionized water, and prepare a dilute sulfuric acid solution with a mass concentration of 1.5% for standby;

[0074] Step (3), preparation of a blank sample reaction vessel: Take 6.0 g of the sodium sulfide solution from step (2) and add it to the reaction vessel, then add 100 g of deionized water. After obtaining a uniform solution, add 1.1 ml of the dilute sulfuric acid solution, and then quickly cover the upper sealing cover. Keep the reaction vessel at a constant temperature of 50 °C, shake well and react to obtain a blank sample reaction vessel;

[0075] Step (3), preparation of a test sample reaction vessel: Under exactly the same conditions as in step (3), prepare a test sample reaction vessel. After shaking well and reacting, use a syringe to inject 100 μL of a liquid desulfurizer (preferably a triazine-based liquid desulfurizer) into the test sample reaction vessel through the sealing plug, shake well, and carry out a desulfurization reaction at a constant temperature of 50 °C for 30 min to obtain a test sample reaction vessel;

[0076] Step (4), detection of hydrogen sulfide gas concentration: After the reactions in the blank sample reaction vessel and the test sample reaction vessel are sufficient, use a hydrogen sulfide detection tube to test the hydrogen sulfide gas concentration in the blank sample reaction vessel to obtain the hydrogen sulfide concentration M0 in the blank sample reaction vessel; Use a hydrogen sulfide detection tube to test the hydrogen sulfide gas concentration in the test sample reaction vessel to obtain the hydrogen sulfide concentration M1 in the test sample reaction vessel;

[0077] Step (5), calculation of the desulfurization rate of the test sample liquid desulfurizer:

[0078]

[0079] Wherein, X is the desulfurization rate, M0 is the concentration of hydrogen sulfide in the blank sample reaction vessel obtained in step (4), in mg / L, and M1 is the concentration of hydrogen sulfide in the test sample reaction vessel obtained in step (4), in mg / L. The desulfurization rate in the test sample reactor is 97%.

[0080] As described above, only the specific embodiments of the present invention are provided, but the protection scope of the present invention is not limited thereto. Any person skilled in the art within the technical scope disclosed by the present invention can easily think of changes or substitutions, which should all be covered within the protection scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.

Claims

1. A method for detecting the desulfurization rate of a liquid desulfurizer product under high-temperature conditions using a detection device, characterized in that, It includes the following steps: Step (1), preparation of the desulfurization detection device: Install the desulfurization detection device as required. The sealing upper cover, sealing bottle stopper, conduit, and sealing clip are all installed as required to form a sealed environment inside the reaction vessel. After detecting the airtightness of the desulfurization detection device, it is ready for use; Step (2), preparation of chemical reagents: Weigh Na2S·9H2O, add deionized water, and prepare a sodium sulfide solution with a mass concentration of 0.1 - 10% for later use; Weigh concentrated sulfuric acid with a concentration of 98%, add deionized water, and prepare a dilute sulfuric acid solution with a mass concentration of 0.5 - 5% for later use; Step (3), preparation of the blank sample reaction vessel: Add 2.0 - 10 g of the sodium sulfide solution from step (2) to the reaction vessel, then add 80 - 200 g of deionized water. After obtaining a homogeneous solution, add 0.1 - 5 ml of the dilute sulfuric acid solution, and then quickly cover the sealing upper cover. Keep the reaction vessel at a constant temperature, shake well and react to obtain the blank sample reaction vessel; Step (3), preparation of the test sample reaction vessel: Under exactly the same conditions as in step (3), prepare the test sample reaction vessel. After shaking well and reacting, use a syringe to inject a measured amount of liquid desulfurizer into the test sample reaction vessel through the sealing plug, shake well and carry out the desulfurization reaction to obtain the test sample reaction vessel; Step (4), detection of hydrogen sulfide gas concentration: After the reactions in the blank sample reaction vessel and the test sample reaction vessel are sufficient, use a hydrogen sulfide detection tube to test the hydrogen sulfide gas concentration in the blank sample reaction vessel to obtain the hydrogen sulfide concentration M0 in the blank sample reaction vessel; Use a hydrogen sulfide detection tube to test the hydrogen sulfide gas concentration in the test sample reaction vessel to obtain the hydrogen sulfide concentration M1 in the test sample reaction vessel; Step (5), calculation of the desulfurization rate of the test sample liquid desulfurizer: In the formula, X is the desulfurization rate, M0 is the hydrogen sulfide concentration in the blank sample reaction vessel obtained in step (4), in mg / L, and M1 is the hydrogen sulfide concentration in the test sample reaction vessel obtained in step (4), in mg / L; The detection device includes a reaction vessel, a sealing upper cover, a sealing bottle stopper, a conduit, and a sealing clip; The sealing upper cover is located at the upper opening of the reaction vessel and is used to form a sealed reaction environment for the reaction vessel; The sealing upper cover is provided with a through hole for the conduit to pass through and an opening for placing the sealing bottle stopper; The conduit passes through the through hole and extends into the reaction vessel to a position in the middle of the reaction vessel, and a sealed condition is maintained between the conduit and the through hole; The sealing clip is clamped at one end of the conduit exposed outside the reaction vessel to seal the part of the conduit communicating with the outside.

2. The method according to claim 1, wherein In step (2), weigh 1.0 g of Na2S·9H2O, add deionized water, and prepare a sodium sulfide solution with a mass concentration of 1% for later use.

3. The method according to claim 1 or 2, characterized in that, In step (2), 1.53 g of concentrated sulfuric acid with a concentration of 98% is weighed, and 98.47 g of deionized water is added to prepare a dilute sulfuric acid solution with a mass concentration of 1.5% for use.

4. The method according to claim 3, characterized in that In step (3), 6 g of the sodium sulfide solution obtained in step (2) is added to a 500 ml reaction vessel, and then 100 g of deionized water is added. After obtaining a homogeneous solution, 0.64 ml of the dilute sulfuric acid solution with a mass concentration of 1.5% is added.

5. The method according to claim 4, wherein In step (3), the sealing cover is quickly covered, and the reaction vessel is kept at a constant temperature of 50 °C.

6. The method according to claim 1, wherein The reaction vessel is a reaction wide-mouth bottle.

7. The method according to claim 1 or 6, characterized in that, The sealing bottle stopper is a rubber bottle stopper.

8. The method according to claim 1, wherein The conduit is a rubber conduit.

9. The method according to claim 1, characterized in that, The sealing clip is a conduit clip.

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