Continuous detection device and method for total sulfur in gas

Abstract

The invention belongs to the field of photoelectric analysis, and particularly relates to a continuous detection method and device for total sulfur in gas, and the detection device comprises a flow control unit and a detection unit; the port of the multi-way valve is respectively communicated with the flow control unit, the quantification unit, the first switching module and the second switching module; the first switching module is used for enabling the first port of the multi-way valve to selectively communicate with the detection unit and the discharge port; the second switching module is used for enabling a second port of the multi-way valve to selectively communicate with a pipeline and a discharge port, and the pipeline is used for communicating the first switching module and a detection unit; and the calculation unit obtains a flow correction value of the gas to be detected according to an output signal of the detection unit. The method has the advantages of continuous detection, accurate detection and the like, and is applied to industries such as natural gas, coal chemical industry and metallurgy.

Description

Technical Field

[0001] The present invention relates to photoelectric analysis, and particularly to a continuous detection device and method for total sulfur in gas. Background Art

[0002] The content of trace total sulfur in industries such as natural gas, coal chemical industry, metallurgy, food, and carbon capture is an important indicator. The content of total sulfur has an important impact on the control of desulfurization process and the quality control of downstream products. By online monitoring the sulfur content in process gas, production can be guided and product quality can be improved.

[0003] At present, most of the methods for detecting total sulfur in gas are non - continuous detections, including lead acetate paper tape method, gas chromatography, and ultraviolet fluorescence method (quantitative loop injection), and real - time continuous detection of total sulfur in gas cannot be achieved. Summary of the Invention

[0004] To solve the deficiencies in the above - mentioned prior art solutions, the present invention provides a continuous detection method for total sulfur in gas.

[0005] The object of the present invention is achieved by the following technical solutions: A continuous detection method for total sulfur in gas includes a detection stage; the continuous detection method further includes a flow rate correction stage, and the flow rate correction stage is as follows: A standard gas with a concentration of C 01 enters a multi - way valve at a flow rate of Q 1 and is quantified by a quantification unit; A carrier gas enters the multi - way valve, pushes the standard gas in the quantification unit into a detection unit, and the detection unit outputs a signal D 01i within a period t; A standard gas with a concentration of C 02 enters the multi - way valve at a flow rate of Q 1 , C 02 ≠C 01 ; The carrier gas enters the multi - way valve, pushes the standard gas in the quantification unit into the detection unit, and the detection unit outputs a signal D 02i within a period t; A gas to be measured enters the multi - way valve at a flow rate of Q 2 and is quantified by the quantification unit; The carrier gas enters the multi - way valve, pushes the standard gas in the quantification unit into the detection unit, and the detection unit outputs a signal D 21i within a period t; A standard gas with a concentration of C 01 successively passes through the multi - way valve and the quantification unit, enters the detection unit, and the detection unit outputs a signal D 1 ; 11 ; Standard gas with a concentration of C 02 flows through the multi-way valve and the metering unit in sequence at a flow rate of Q 1 and enters the detection unit. The detection unit outputs signal D 12 ; The gas to be measured flows through the multi-way valve and the metering unit in sequence at a flow rate of Q 2 and enters the detection unit. The detection unit outputs signal D 22 ; Adjust the target flow rate Q of the gas to be measured to: ; In the detection stage, the gas to be measured continuously enters the multi-way valve, the metering unit and the detection unit at a flow rate of Q, and the detection unit outputs the total sulfur content.

[0006] The object of the present invention also lies in providing a continuous detection device for total sulfur in gas, and this object of the invention is achieved through the following technical solutions.

[0007] A continuous detection device for total sulfur in gas includes a flow control unit and a detection unit; the continuous detection device further includes: A multi-way valve and a metering unit, the ports of the multi-way valve are respectively connected to the flow control unit, the metering unit, the first switching module and the second switching module; when the multi-way valve switches to the first state, the gas passing through the flow control unit enters the multi-way valve, and sequentially passes through the metering unit and the first port of the multi-way valve, when the multi-way valve switches to the second state, the gas passing through the flow control unit enters the multi-way valve, and sequentially passes through the metering unit and the second port of the multi-way valve; A first switching module, the first switching module is used to selectively connect the first port of the multi-way valve to the detection unit and the discharge port; A second switching module, the second switching module is used to selectively connect the second port of the multi-way valve to the pipeline and the discharge port, and the pipeline is used to connect the first switching module and the detection unit; A calculation unit, the calculation unit obtains the flow correction value of the gas to be measured according to the output signal of the detection unit.

[0008] Compared with the prior art, the beneficial effects of the present invention are: Solve the problem that the current total sulfur meter can only measure intermittently, and automatically correct the calibration coefficient of the flow rate of the gas to be measured, without knowing the composition of the gas to be measured, so as to adapt to the precise control of the flow rate of gases with different working conditions and different compositions, and thus realize the real-time continuous monitoring of the total sulfur concentration of the gas. Description of the Drawings

[0009] With reference to the accompanying drawings, the disclosure of the present invention will become more readily understandable. It is readily understandable to those skilled in the art that these drawings are merely for illustrative purposes of the technical solutions of the present invention and are not intended to limit the scope of protection of the present invention. In the drawings: Figure 1 is a schematic structural diagram of a continuous detection device for total sulfur in a gas of the present invention. Detailed implementation manners

[0010] Figure 1 The following description and the following illustrate alternative specific embodiments of the present invention to teach those skilled in the art how to implement and reproduce the present invention. For the purpose of teaching the technical solutions of the present invention, some conventional aspects have been simplified or omitted. Those skilled in the art should understand that variations or substitutions derived from these specific embodiments will fall within the scope of the present invention. Those skilled in the art should understand that the following features can be combined in various ways to form multiple variations of the present invention. Thus, the present invention is not limited to the following alternative specific embodiments, but is defined only by the claims and their equivalents.

[0011] Example 1.

[0012] A continuous detection device for total sulfur in a gas, as Figure 1 shown, includes: a flow control unit 11 and a detection unit.

[0013] The ports of the multi-way valve 21 are respectively connected to the flow control unit 11, the metering unit 22, the first switching module 42, and the second switching module 41; when the multi-way valve 21 is switched to the first state, the gas passing through the flow control unit 11 enters the multi-way valve 21 and sequentially passes through the metering unit 22 and the first port 211 of the multi-way valve 21. When the multi-way valve 21 is switched to the second state, the gas passing through the flow control unit 11 enters the multi-way valve 21 and sequentially passes through the metering unit 22 and the second port 212 of the multi-way valve 21.

[0014] The first switching module 42 is used to selectively connect the first port 211 of the multi-way valve 21 to the detection unit and the discharge port 51.

[0015] The second switching module 41 is used to selectively connect the second port 212 of the multi-way valve 21 to a pipeline and the discharge port 51, and the pipeline is used to connect the first switching module 42 and the detection unit.

[0016] The calculation unit 61 obtains a flow correction value of the gas to be measured according to the output signal of the detection unit.

[0017] In order to accurately detect total sulfur, further, the detection unit includes: a conversion module 31 for converting sulfur in the gas into sulfur dioxide.

[0018] The detection module 33 detects the sulfur dioxide content.

[0019] To improve the conversion efficiency and thus the total sulfur detection accuracy, further, the conversion module 31 employs a combustion furnace, and the combustion-supporting gas and the auxiliary gas are connected to the conversion module 31 after flow control.

[0020] A continuous detection method for total sulfur in a gas according to an embodiment of the present invention, that is, the working method of the detection device in this example, the continuous detection method includes a detection stage, and the continuous detection method further includes a flow rate correction stage, and the flow rate correction stage is as follows: A standard gas with a concentration of C 01 enters the multi-way valve 21 at a flow rate of Q 1 and is quantified by the quantification unit 22.

[0021] The carrier gas enters the multi-way valve 21, pushes the standard gas in the quantification unit 22 into the detection unit, and the detection unit outputs a signal D within a period t 01i .

[0022] A standard gas with a concentration of C 02 enters the multi-way valve 21 at a flow rate of Q 1 , and C 02 ≠C 01 .

[0023] The carrier gas enters the multi-way valve 21, pushes the standard gas in the quantification unit 22 into the detection unit, and the detection unit outputs a signal D within a period t 02i .

[0024] The gas to be measured enters the multi-way valve 21 at a flow rate of Q 2 and is quantified by the quantification unit 22.

[0025] The carrier gas enters the multi-way valve 21, pushes the gas to be measured in the quantification unit 22 into the detection unit, and the detection unit outputs a signal D within a period t 21i .

[0026] A standard gas with a concentration of C 01 enters the detection unit by sequentially passing through the multi-way valve 21 and the quantification unit 22 at a flow rate of Q 1 , and the detection unit outputs a signal D 11 .

[0027] A standard gas with a concentration of C 02 enters the detection unit by sequentially passing through the multi-way valve 21 and the quantification unit 22 at a flow rate of Q 1 , and the detection unit outputs a signal D 12 .

[0028] The gas to be measured enters the detection unit through the multi-way valve 21 and the metering unit 22 in sequence at a flow rate of Q 2 and outputs a signal D 22 .

[0029] The target flow rate Q of the gas to be measured is adjusted to: .

[0030] In the detection stage, the gas to be measured continuously enters the multi-way valve 21, the metering unit 22 and the detection unit at a flow rate of Q, and the detection unit outputs the total sulfur content

[0031] To improve reliability, further, the multi-way valve 21 adopts a switching valve, both ends of the flow control unit 11 are connected to the ports of the switching valve, and the metered carrier gas, standard gas and gas to be measured are respectively connected to the ports of the switching valve

[0032] In the above detection method, during the metering of the metering unit 22, the first switching module 42, the second switching module 41 and the switching valve switch. The first switching module 42 disconnects the connection with the detection unit, and the second switching module 41 disconnects the connection with the detection unit. The gas passes through the first port 211 of the switching valve and the first switching module 42 in sequence and enters the discharge port 51 When obtaining D 01i , D 02i and D 21i , the first switching module 42, the second switching module 41 and the switching valve switch. The first switching module 42 disconnects the connection with the detection unit, and the gas passes through the second port 212 of the switching valve and the second switching module 41 in sequence and enters the pipeline between the first switching module 42 and the detection unit, and then enters the detection unit When obtaining D 11 , D 12 and D 22 , the first switching module 42, the second switching module 41 and the switching valve switch. The second switching module 41 disconnects the connection with the detection unit, and the gas passes through the first port 211 of the switching valve, the first switching module 42 and the detection unit in sequence

[0033] Embodiment 2

[0034] An application example of the continuous detection device and method for total sulfur in gas according to Embodiment 1 of the present invention

[0035] In this application example, the carrier gas, the gas to be measured, the standard gas, the combustion-supporting gas and the auxiliary gas are respectively connected to the flow control unit 11. Among them, valves are respectively arranged on the flow paths of the gas to be measured and the standard gas, and they are combined into one path and enter the flow control unit. After that, the combustion-supporting gas and the auxiliary gas after flow control are sent to the conversion module 31, and the carrier gas and the gas to be measured (or the standard gas) are sent to the multi-way valve 21

[0036] The multi-way valve 21 is a six-way valve and can be switched to a first state or a second state. When the multi-way valve 21 is switched to the first state, the gas passing through the flow control unit 11 enters the multi-way valve 21 and sequentially passes through the metering unit 22 and the first port 211 of the multi-way valve 21. When the multi-way valve 21 is switched to the second state, the gas passing through the flow control unit 11 enters the multi-way valve 21 and sequentially passes through the metering unit 22 and the second port 212 of the multi-way valve 21.

[0037] The first switching module 42 is used to selectively connect the first port 211 of the multi-way valve 21 to the detection unit and the discharge port 51. The second switching module 41 is used to selectively connect the second port 212 of the multi-way valve 21 to the pipeline and the discharge port 51, and the pipeline is used to connect the first switching module 42 and the detection unit. The first switching module 42 and the second switching module 41 respectively adopt electromagnetic three-way valves.

[0038] The detection unit includes a conversion module, a water removal module and a detection module connected in sequence. The conversion module adopts a high-temperature combustion furnace, specifically a quartz combustion tube at 1050 ± 50 °C. Sulfides and O in the gas to be measured 2 are completely oxidized to generate SO under high-temperature oxygen-rich conditions at 1100 °C 2 . The three-way gases of the gas to be measured, the combustion-supporting gas and the auxiliary gas continuously enter the high-temperature combustion furnace through the flow control unit 11, and the sulfides in the gas to be measured are continuously oxidized to generate SO 2 , so as to realize continuous detection. The detection module 33 adopts an ultraviolet fluorescence detection module.

[0039] The calculation unit 61 obtains the flow correction value of the gas to be measured according to the output signal of the detection unit. The specific calculation method is shown in the detection method section.

[0040] A continuous detection method for total sulfur in a gas, that is, the working method of the detection device in this example. The continuous detection method includes a detection stage, and the continuous detection method also includes a flow correction stage. The flow correction stage is as follows: The standard gas with a concentration of C 01 (the standard gas contains a total sulfur concentration of 0 mg / Nm 3 ) enters the multi-way valve 21 at a flow rate of Q 1 (10 mL / min) and is metered by the metering unit 22 (the metering volume is 300 μL).

[0041] The carrier gas (flow rate 200 mL / min) enters the multi-way valve 21, pushes the standard gas in the metering unit 22 into the detection unit, and the detection unit outputs a signal D within the period t 01i .

[0042] The standard gas with a concentration of C02 The calibration gas (the calibration gas contains a total sulfur concentration of 400 mg / Nm 3 ) enters the multi-way valve 21 at a flow rate Q 1 (10 mL / min), and is quantified by the quantification unit 22 (quantification volume 300 μL). C 02 ≠C 01 .

[0043] The carrier gas (flow rate 200 mL / min) enters the multi-way valve 21, pushes the calibration gas in the quantification unit 22 into the detection unit, and the detection unit outputs a signal D within the period t 02i .

[0044] The gas to be measured enters the multi-way valve 21 at a flow rate Q 2 (10 mL / min), and is quantified by the quantification unit 22 (quantification volume 300 μL).

[0045] The carrier gas (flow rate 200 mL / min) enters the multi-way valve 21, pushes the gas to be measured in the quantification unit 22 into the detection unit, and the detection unit outputs a signal D within the period t 21i .

[0046] The calibration gas with a concentration of C 01 (the calibration gas contains a total sulfur concentration of 0 mg / Nm 3 ) enters the detection unit by passing through the multi-way valve 21 and the quantification unit 22 in sequence at a flow rate Q 1 (10 mL / min), and the detection unit outputs a signal D 11 (0 mg / Nm 3 ).

[0047] The calibration gas with a concentration of C 02 (the calibration gas contains a total sulfur concentration of 400 mg / Nm 3 ) enters the detection unit by passing through the multi-way valve 21 and the quantification unit 22 in sequence at a flow rate Q 1 (10 ml / min), and the detection unit outputs a signal D 12 (400 mg / Nm 3 ).

[0048] The gas to be measured enters the detection unit by passing through the multi-way valve 21 and the quantification unit 22 in sequence at a flow rate Q 2 (10 mL / min), and the detection unit outputs a signal D 22 (1200 mg / Nm 3 ).

[0049] Adjust the target flow rate Q of the gas to be measured to: .

[0050] In the detection stage, the gas to be measured continuously enters the multi-way valve 21, the metering unit 22 and the detection unit at a flow rate Q, and the detection unit outputs the total sulfur content (300 mg / Nm 3 ).

[0051] In the quantification of the metering unit 22 in the above detection method, the first switching module 42, the second switching module 41 and the switching valve switch. The first switching module 42 disconnects the connection with the detection unit, and the second switching module 41 disconnects the connection with the detection unit. The gas sequentially passes through the first port 211 of the switching valve and the first switching module 42 and enters the discharge port 51.

[0052] When obtaining D 01i , D 02i and D 21i , the first switching module 42, the second switching module 41 and the switching valve switch. The first switching module 42 disconnects the connection with the detection unit. The gas sequentially passes through the second port 212 of the switching valve and the second switching module 41, enters the pipeline between the first switching module 42 and the detection unit, and then enters the detection unit.

[0053] When obtaining D 11 , D 12 and D 22 , the first switching module 42, the second switching module 41 and the switching valve switch. The second switching module 41 disconnects the connection with the detection unit. The gas sequentially passes through the first port 211 of the switching valve, the first switching module 42 and the detection unit.

[0054] In the above detection method, the target flow rate of the carrier gas (gas types are air, nitrogen, oxygen, etc.) is 200 ml / min, the target flow rate of the gas to be measured is 20 ml / min, the target flow rate of the combustion-supporting gas is 200 ml / min (gas types are air or oxygen, etc.), and the target flow rate of the auxiliary gas (gas types are air or nitrogen, etc.) is 800 ml / min. Connect the carrier gas, combustion-supporting gas and auxiliary gas gas sources, and turn on these three gas sources.

Claims

1. A method for continuous detection of total sulfur in gas, comprising a detection stage; characterized in that: The continuous detection method further comprises a flow correction stage, which comprises: The concentration is C 01 The standard gas enters the multi-way valve at a flow rate of Q1 and is quantified by the quantitative unit; The carrier gas enters the multi-way valve, pushing the standard gas in the quantitative unit into the detection unit. The detection unit outputs a signal D in period t. 01i ; The concentration is C 02 The standard gas enters the multi-way valve at a flow rate of Q1 and is quantitatively measured by the quantitative unit, C 02 ≠C 01 ; The carrier gas enters the multi-way valve, pushing the standard gas in the quantitative unit into the detection unit. The detection unit outputs a signal D in period t. 02i ; The gas to be tested enters the multi-way valve at a flow rate of Q2 and is quantified using a quantitative unit; The carrier gas enters the multi-way valve, pushing the standard gas in the quantitative unit into the detection unit. The detection unit outputs a signal D in period t. 21i ; The concentration is C 01 The standard gas passes through the multi-way valve and the quantitative unit in sequence at a flow rate of Q1 and enters the detection unit. The detection unit outputs a signal D 11 ; The concentration is C 02 The standard gas passes through the multi-way valve and the quantitative unit in sequence at a flow rate of Q1 and enters the detection unit. The detection unit outputs a signal D 12 ; The gas to be tested passes through the multi-way valve and the quantitative unit in sequence at a flow rate of Q2 and enters the detection unit. The detection unit outputs a signal D 22 ; Adjust the target flow rate Q of the gas to be tested to: ； In the detection stage, the gas to be detected continuously enters the multi-way valve, the quantitative unit and the detection unit at a flow rate Q, and the detection unit outputs the total sulfur content.

2. The method for continuous detection of total sulfur in gas according to claim 1, characterized in that: The multi-way valve adopts a switching valve, and both ends of the flow control unit are connected to the ports of the switching valve. The quantitative carrier gas, standard gas and gas to be tested are respectively connected to the ports of the switching valve.

3. The method for continuous detection of total sulfur in gas according to claim 2, characterized in that: During the quantitative measurement of the quantitative unit, the first switching module, the second switching module and the switching valve are switched, the first switching module is disconnected from the connection with the detection unit, the second switching module is disconnected from the connection with the detection unit, and the gas passes through the first port of the switching valve and the first switching module in sequence and enters the discharge port; In getting D 01i , D 02i and D 21i In the process, the first switching module, the second switching module and the switching valve are switched, the first switching module is disconnected from the detection unit, and the gas passes through the second port of the switching valve and the second switching module in sequence, enters the pipeline between the first switching module and the detection unit, and then enters the detection unit; In getting D 11 , D 12 and D 22 In the process, the first switching module, the second switching module and the switching valve are switched, the second switching module is disconnected from the detection unit, and the gas passes through the first port of the switching valve, the first switching module and the detection unit in sequence.

4. The method for continuous detection of total sulfur in gas according to claim 1, characterized in that: The detection unit comprises: A conversion module, the conversion module is used to convert sulfur in the gas into sulfur dioxide; A detection module is used to detect sulfur dioxide content.

5. The method for continuous detection of total sulfur in gas according to claim 4, characterized in that: The conversion module adopts a combustion furnace, and the combustion-supporting gas and the auxiliary gas are connected to the conversion module after flow control.

6. A continuous detection device for total sulfur in gas, comprising a flow control unit and a detection unit; characterized in that: The continuous detection device also includes: A multi-way valve and a quantitative unit, wherein the ports of the multi-way valve are respectively connected to the flow control unit, the quantitative unit, the first switching module and the second switching module; when the multi-way valve is switched to the first state, the gas passing through the flow control unit enters the multi-way valve, passes through the quantitative unit and the first port of the multi-way valve in sequence; when the multi-way valve is switched to the second state, the gas passing through the flow control unit enters the multi-way valve, passes through the quantitative unit and the second port of the multi-way valve in sequence; a first switching module, the first switching module being used to selectively connect the first port of the multi-way valve to the detection unit and the discharge port; A second switching module, the second switching module is used to selectively connect the second port of the multi-way valve to a pipeline and a discharge port, the pipeline is used to connect the first switching module and the detection unit; A calculation unit is used to obtain a flow correction value of the gas to be measured according to the output signal of the detection unit.

7. The continuous detection device for total sulfur in gas according to claim 6, characterized in that: The detection unit comprises: A conversion module, the conversion module is used to convert sulfur in the gas into sulfur dioxide; A detection module is used to detect sulfur dioxide content.

8. The continuous detection device for total sulfur in gas according to claim 7, characterized in that: The conversion module adopts a combustion furnace, and the combustion-supporting gas and the auxiliary gas are connected to the conversion module after flow control.

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