CN103308515A - Online analysis system and method for detection of CO gas at ammonia synthesis inlet - Google Patents
Online analysis system and method for detection of CO gas at ammonia synthesis inlet Download PDFInfo
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- CN103308515A CN103308515A CN2013101827036A CN201310182703A CN103308515A CN 103308515 A CN103308515 A CN 103308515A CN 2013101827036 A CN2013101827036 A CN 2013101827036A CN 201310182703 A CN201310182703 A CN 201310182703A CN 103308515 A CN103308515 A CN 103308515A
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- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 title claims abstract description 66
- 238000004458 analytical method Methods 0.000 title claims abstract description 43
- 229910021529 ammonia Inorganic materials 0.000 title claims abstract description 33
- 238000003786 synthesis reaction Methods 0.000 title claims abstract description 33
- 230000015572 biosynthetic process Effects 0.000 title claims abstract description 32
- 238000001514 detection method Methods 0.000 title claims abstract description 11
- 238000000034 method Methods 0.000 title description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 21
- 238000005070 sampling Methods 0.000 claims abstract description 14
- 238000005406 washing Methods 0.000 claims abstract description 7
- 238000004868 gas analysis Methods 0.000 claims abstract description 5
- 230000000087 stabilizing effect Effects 0.000 claims description 7
- 238000002203 pretreatment Methods 0.000 claims 1
- 238000001914 filtration Methods 0.000 abstract description 4
- 238000005259 measurement Methods 0.000 abstract description 4
- 238000006477 desulfuration reaction Methods 0.000 abstract description 2
- 230000023556 desulfurization Effects 0.000 abstract description 2
- 238000001035 drying Methods 0.000 abstract description 2
- 238000004445 quantitative analysis Methods 0.000 abstract description 2
- 239000007789 gas Substances 0.000 description 80
- 239000003054 catalyst Substances 0.000 description 9
- 238000012544 monitoring process Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 231100000572 poisoning Toxicity 0.000 description 4
- 230000000607 poisoning effect Effects 0.000 description 4
- 239000000428 dust Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 239000004793 Polystyrene Substances 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 229920002223 polystyrene Polymers 0.000 description 2
- XTQHKBHJIVJGKJ-UHFFFAOYSA-N sulfur monoxide Chemical class S=O XTQHKBHJIVJGKJ-UHFFFAOYSA-N 0.000 description 2
- 229910052815 sulfur oxide Inorganic materials 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 235000019738 Limestone Nutrition 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000006028 limestone Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 238000007781 pre-processing Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
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Abstract
unit which are sequentially connected, wherein the sampling unit feeds pressure-constant gas into the pretreatment unit through a double-flange high-pressure cut-off valve and a water seal, and then the unit which are sequentially connected, wherein the sampling unit feeds pressure-constant gas into the pretreatment unit through a double-flange high-pressure cut-off valve and a water seal, and then the pressure-constant gas is fed into the gas analysis unit. Sampled gas is automatically subjected to washing, drying and desulfurization, fine filtration, and flow measurement and quantitative analysis. A gas analyzer is subjected to zero calibration and measuring range calibration through standard gas connected at the analysis unit, thereby realizing the online calibration of the analysis system. The invention also discloses an online analysis method for the detection of CO gas at an ammonia synthesis inlet. Through the online analysis system disclosed by the invention, the accurate, reliable and online detection and analysis on the content of CO gas at an ammonia synthesis inlet can be realized.
Description
Technical Field
The invention relates to an online real-time monitoring system, in particular to an online analysis system, which is used for monitoring the content of CO gas at an ammonia synthesis inlet in real time.
Background
In the ammonia synthesis production process, a catalyst is a main synthesis vehicle, the activity degree of the catalyst directly influences the yield of ammonia, but the activity of the catalyst is usually obviously reduced or even destroyed due to the contact of a small amount of impurities during the stable activity period, and the phenomenon is called catalyst poisoning, and the poisoning is generally considered to be caused because active centers on the surface of the catalyst are occupied by the impurities. For example, in the case of iron catalysts in ammonia synthesis reactions, CO2, O2, water vapor, etc. can all cause catalyst poisoning, and even if pure hydrogen and nitrogen mixed gas can recover its activity, the performance of the catalyst can be severely degraded. Therefore, there is a need for real-time monitoring of ammonia synthesis inlet gas composition to prevent catalyst poisoning, thereby ensuring efficient and stable operation of the ammonia synthesis system.
At present, most ammonia synthesis plants mainly adopt a method for detecting ammonia synthesis inlet gas by off-line sampling, then detecting the gas in a laboratory and controlling a front section, so that the real-time monitoring cannot be realized, and the error is very high. Therefore, a special detection processing system needs to be constructed for these aspects.
Disclosure of Invention
The invention aims to provide an online analysis system for detecting CO gas at an ammonia synthesis inlet, which is used for timely processing and analyzing the CO content of the ammonia synthesis inlet gas.
Another purpose of the invention is to provide an online analysis method for detecting CO gas at an ammonia synthesis inlet, which can timely process and analyze the CO content of the ammonia synthesis inlet gas.
The technical scheme adopted by the invention is as follows:
the online analysis system for detecting the CO gas at the ammonia synthesis inlet comprises a sampling unit, a pretreatment unit, an analysis unit and a calibration unit which are sequentially connected.
The sampling unit comprises a double-flange high-pressure stop valve, a water seal, a first ball valve and a second ball valve, wherein the first ball valve is arranged on a pipeline entering the water seal, and the second ball valve is arranged on an outlet pipeline of the water seal. And the pressure of the fresh gas of 22MPa is reduced by the double-flange stop valve, and then the fresh gas passes through the ball valve to enter the water seal, so that the stability of the gas is ensured.
The pretreatment unit comprises a washing bottle, a dryer, a desulfurizer and a filter which are connected in sequence. Wherein, the water washing bottle is used for removing large particles in the gas and other liquid in the gas; the dryer is used for removing moisture in the gas; the desulfurizer is used for removing sulfur oxides and H in gas2S and other harmful gases; the filter adopts a polystyrene film filter element for secondary fine filtration to remove small-particle dust.
The analysis unit comprises a pressure stabilizing valve, a pressure gauge, a four-way valve, a flowmeter and a gas analyzer which are connected in sequence. The pressure stabilizing valve is of a conical valve core type, has a self-regulating function on inlet pressure, and then enters the gas analyzer through the four-way valve and the flowmeter.
In order to facilitate the online calibration of the gas analyzer in the analysis unit, the online analysis system for detecting the CO gas at the ammonia synthesis inlet also comprises a calibration unit. The calibration unit is connected with the analysis unit.
The calibration unit comprises a zero standard gas cylinder with a pressure reducing valve and a measuring range standard gas cylinder with a pressure reducing valve. The zero standard gas cylinder and the measuring range standard gas cylinder are respectively connected with a four-way valve of the analysis unit through a pressure reducing valve arranged on the zero standard gas cylinder and the measuring range standard gas cylinder, and when the gas analyzer needs to be calibrated, the four-way valve is used for switching.
The invention also discloses an online analysis method for detecting CO gas at an ammonia synthesis inlet, which comprises the following steps:
1) gas sampling: the pressure of fresh gas of 22MPa is reduced by a double-flange stop valve, and then the fresh gas enters a water seal through a ball valve;
2) gas pretreatment: the gas from the water seal is sequentially led into a washing bottle, a dryer, a desulfurizer and a filter;
3) and (3) gas analysis: and (3) after the sampled gas is treated in the step 2), introducing the sampled gas into a pressure stabilizing valve for pressure regulation, sending the sampled gas into a flow meter through a four-way valve for gas flow regulation, and finally, sending the gas into a gas analyzer.
In order to facilitate the online calibration of the gas analyzer, the online analysis method for detecting the CO gas at the ammonia synthesis inlet also comprises a gas calibration step. And through the switching of the four-way valve, gas in the zero standard gas cylinder or the range standard gas cylinder is communicated with the pipeline to calibrate the gas analyzer.
The gas analyzer of the invention is an infrared gas analyzer.
The technical scheme of the invention has the following beneficial effects:
the invention discloses an online analysis system for detecting CO gas at an ammonia synthesis inlet, which comprises a sampling unit, a pretreatment unit, an analysis unit and a calibration unit which are sequentially connected. And the sampled gas is automatically subjected to washing, drying, desulfurization, fine filtration, flow metering and quantitative analysis. And the gas analyzer is subjected to zero calibration and range calibration through the standard gas connected with the analysis unit, so that the online calibration of the analysis system is realized. The invention also discloses an online analysis method for detecting the CO gas at the ammonia synthesis inlet. The online analysis system can realize accurate, reliable and online detection and analysis of the CO content of the ammonia synthesis inlet gas.
The invention discloses an online analysis method for detecting CO gas at an ammonia synthesis inlet, which comprises the steps of gas sampling, gas pretreatment, gas analysis and the like. After the pressure of fresh gas of 22MPa is reduced by the double-flange high-pressure stop valve, the fresh gas passes through the ball valve and enters the water seal, so that the stability of the gas is ensured. The pre-processing unit and the re-processing step before gas analysis make the gas detection data more accurate and reliable. Through the switching of the four-way valve, the online calibration of the gas analyzer is realized, the calibration process is simplified, and the continuity of the monitoring process is improved.
Drawings
FIG. 1 is a schematic structural diagram of an embodiment of an on-line analysis system for detecting CO gas at an ammonia synthesis inlet according to the present invention.
Detailed Description
The technical scheme of the invention is described in detail in the following with reference to the accompanying drawings.
As shown in FIG. 1, the online analysis system for detecting CO gas at an ammonia synthesis inlet comprises a sampling unit 1, a pretreatment unit 2, an analysis unit 3 and a calibration unit 4 which are connected in sequence.
The sampling unit 1 comprises a double-flange high-pressure stop valve 12, a ball valve 13, a ball valve 14, a ball valve 16 and a water seal 15; the two ball valves 13 are respectively arranged at the air inlet and the air outlet of the water seal, and the ball valve 14 and the ball valve 16 are a water injection valve and a sewage valve of the water seal. In the embodiment, the double-flange high-pressure stop valve 12 is in a model number of J44H-320P.
The pretreatment unit 2 includes a wash bottle 22, a dryer 23, a desulfurizer 24, and a filter 25, which are connected in this order. In this embodiment, the water wash bottle 22 is a conventional chemical reagent glass bottle for removing dust and other liquids in gases having a particle size of 20 microns or more. Model numbers of the dryer 23 and the desulfurizer 24 are FT-2 (Nanjing Xin)Branch measurement and control instrument limited), a dryer 23 is filled with silica gel for removing moisture in gas, and a desulfurizer 24 is filled with limestone for removing sulfur oxides and H in gas2S and the like. The filter 25 is of type FF-1 (Nanjing Xinfen measurement and control instrument Co., Ltd.) and uses a polystyrene film filter core for secondary fine filtration to remove small-particle dust. After the gas passes through the pretreatment unit 2 through the sampling unit 1, the corrosion of harmful components in the gas to a gas pipeline and an analyzer can be greatly reduced, and the measurement precision is improved.
The analysis unit comprises a pressure stabilizing valve 35, a pressure gauge 31, a four-way valve 36, a flow meter 33 and a gas analyzer 32 which are connected in sequence. In this embodiment, the pressure stabilizing valve 35 is a conical spool type JTF-2 (Chuanglead scientific instruments, Inc. of Taizhou), and the inlet pressure is self-regulated. The gas analyzer 32 was analyzed using an infrared CO analyzer model QGS-08 (beijing beige haake analyzer ltd).
Calibration unit 4 includes a zero standard gas cylinder 42 with a pressure reducing valve 41 and a span standard gas cylinder 43 with a pressure reducing valve 41. The zero standard gas cylinder 42 and the range standard gas cylinder 43 are connected to the four-way valve 36 of the analysis unit via a pressure reducing valve 41 provided therein, and are switched by the four-way valve 36 when the gas analyzer 32 needs to be calibrated.
Claims (7)
1. An online analysis system for detecting CO gas at an ammonia synthesis inlet is characterized by comprising a sampling unit, a pretreatment unit, an analysis unit and a calibration unit which are sequentially connected; wherein,
the sampling unit comprises a double-flange high-pressure stop valve, a water seal, a first ball valve and a second ball valve, wherein the first ball valve is arranged on a pipeline entering the water seal, and the second ball valve is arranged on an outlet pipeline of the water seal.
2. The on-line analysis system for ammonia synthesis inlet CO gas detection as claimed in claim 1, wherein the pre-treatment unit comprises a washing bottle, a dryer, a desulfurizer and a filter which are connected in sequence.
3. The on-line analysis system for detecting the CO gas at the ammonia synthesis inlet of claim 1, wherein the analysis unit comprises a pressure stabilizing valve, a pressure gauge, a four-way valve, a flow meter and a gas analyzer which are connected in sequence.
4. The on-line analysis system for ammonia synthesis inlet CO gas detection as claimed in claim 1 further comprising a calibration unit connected to the analysis unit.
5. The on-line analysis system for ammonia synthesis inlet CO gas detection as claimed in claim 4 wherein said calibration unit comprises a zero standard gas cylinder with a pressure reducing valve and a span standard gas cylinder with a pressure reducing valve.
6. The on-line analysis system for ammonia synthesis inlet CO gas detection as claimed in claim 5, wherein said calibration unit comprises a zero standard gas cylinder with pressure reducing valve and said range standard gas cylinder with pressure reducing valve, which are respectively connected with said four-way valve in said analysis unit through their respective pressure reducing valves.
7. An on-line analysis system for ammonia synthesis inlet CO gas detection, comprising the steps of:
1) gas sampling: the pressure of fresh gas of 22MPa is reduced by a double-flange stop valve, and then the fresh gas enters a water seal through a ball valve;
2) gas pretreatment: the gas from the water seal is sequentially led into a washing bottle, a dryer, a desulfurizer and a filter;
3) and (3) gas analysis: and (3) after the sampled gas is treated in the step 2), introducing the sampled gas into a pressure stabilizing valve for pressure regulation, sending the sampled gas into a flow meter through a four-way valve for gas flow regulation, and finally, sending the gas into a gas analyzer.
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Cited By (6)
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CN104165882A (en) * | 2014-08-29 | 2014-11-26 | 四川九高科技有限公司 | Gas input device and Raman spectrometer comprising gas input device |
CN104713766A (en) * | 2013-12-13 | 2015-06-17 | 中国石油天然气股份有限公司 | Sample pretreatment method and device for laser Raman natural gas analyzer |
CN105784941A (en) * | 2016-03-23 | 2016-07-20 | 中国科学院光电研究院 | Device and method for analyzing gas in online manner |
CN109856334A (en) * | 2019-02-01 | 2019-06-07 | 中国石油天然气集团公司 | A kind of real-time analytical equipment of gas pipeline hydrogen sulfide |
CN109900860A (en) * | 2019-02-01 | 2019-06-18 | 中国石油天然气集团公司 | A kind of gas pipeline hydrogen sulfide real-time analysis method |
CN111855911A (en) * | 2020-07-29 | 2020-10-30 | 中航长城计量测试(天津)有限公司 | Combustible gas distribution device |
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CN104713766A (en) * | 2013-12-13 | 2015-06-17 | 中国石油天然气股份有限公司 | Sample pretreatment method and device for laser Raman natural gas analyzer |
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Application publication date: 20130918 |