CN113484477A - Detection apparatus for hydrogen chloride content in hydrogenation apparatus gas phase and gas circuit system - Google Patents
Detection apparatus for hydrogen chloride content in hydrogenation apparatus gas phase and gas circuit system Download PDFInfo
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- CN113484477A CN113484477A CN202110805555.3A CN202110805555A CN113484477A CN 113484477 A CN113484477 A CN 113484477A CN 202110805555 A CN202110805555 A CN 202110805555A CN 113484477 A CN113484477 A CN 113484477A
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- 239000007789 gas Substances 0.000 title claims abstract description 107
- 238000001514 detection method Methods 0.000 title claims abstract description 92
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 title claims abstract description 64
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 title claims abstract description 64
- 229910000041 hydrogen chloride Inorganic materials 0.000 title claims abstract description 64
- 238000005984 hydrogenation reaction Methods 0.000 title claims abstract description 56
- 238000010521 absorption reaction Methods 0.000 claims abstract description 99
- 238000001816 cooling Methods 0.000 claims abstract description 34
- 238000005070 sampling Methods 0.000 claims abstract description 23
- 239000007788 liquid Substances 0.000 claims abstract description 19
- 238000004321 preservation Methods 0.000 claims abstract description 8
- 230000005494 condensation Effects 0.000 claims abstract description 5
- 238000009833 condensation Methods 0.000 claims abstract description 5
- 230000001105 regulatory effect Effects 0.000 claims description 29
- 238000007789 sealing Methods 0.000 claims description 11
- 238000005192 partition Methods 0.000 claims description 7
- -1 polytetrafluoroethylene Polymers 0.000 claims description 4
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 4
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 4
- 239000012071 phase Substances 0.000 abstract description 25
- 239000007792 gaseous phase Substances 0.000 abstract description 3
- 239000003208 petroleum Substances 0.000 abstract description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- HIVLDXAAFGCOFU-UHFFFAOYSA-N ammonium hydrosulfide Chemical compound [NH4+].[SH-] HIVLDXAAFGCOFU-UHFFFAOYSA-N 0.000 description 6
- 239000001284 azanium sulfanide Substances 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 6
- 230000007797 corrosion Effects 0.000 description 6
- 238000005260 corrosion Methods 0.000 description 6
- 239000001257 hydrogen Substances 0.000 description 6
- 229910052739 hydrogen Inorganic materials 0.000 description 6
- 239000002250 absorbent Substances 0.000 description 5
- 230000002745 absorbent Effects 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- 239000002253 acid Substances 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 150000002431 hydrogen Chemical class 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 239000003921 oil Substances 0.000 description 4
- 150000003839 salts Chemical class 0.000 description 3
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical class [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 230000002378 acidificating effect Effects 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 239000010779 crude oil Substances 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 239000004809 Teflon Substances 0.000 description 1
- 229920006362 Teflon® Polymers 0.000 description 1
- 239000006096 absorbing agent Substances 0.000 description 1
- 150000003863 ammonium salts Chemical group 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 238000004255 ion exchange chromatography Methods 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/0004—Gaseous mixtures, e.g. polluted air
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/0004—Gaseous mixtures, e.g. polluted air
- G01N33/0009—General constructional details of gas analysers, e.g. portable test equipment
- G01N33/0011—Sample conditioning
- G01N33/0016—Sample conditioning by regulating a physical variable, e.g. pressure or temperature
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Food Science & Technology (AREA)
- Combustion & Propulsion (AREA)
- Physics & Mathematics (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
The embodiment of the invention provides a detection device for hydrogen chloride content in a gas phase of a hydrogenation device and a gas circuit system, and relates to the field of petroleum processing equipment. This detection device of hydrogen chloride content in hydrogenation device gaseous phase is including the detection pipeline that is used for the sampling pipeline intercommunication predetermined with hydrogenation device's gas circuit pipeline, a cooling container that is used for holding the absorption vessel of alkaline absorption liquid and is used for carrying out the condensation to hydrogen chloride in getting into the absorption vessel, the last relief pressure valve that has set gradually of detection pipeline, manometer and flow control valve, the end and the absorption vessel intercommunication of detection pipeline, the absorption vessel sets up in the cooling container, detection pipeline and the cooling container outside all overlap and are equipped with the heat preservation. The detection device can realize the regulation of the pressure and the flow of gas in the detection pipeline, and has wide detection range and high applicability. In addition, this application can effectively avoid the steam in the gas to condense before getting into the absorption vessel, and HCl in the gas can be totally in the absorption vessel condensation, and the testing result is more accurate.
Description
Technical Field
The invention relates to the field of petroleum processing equipment, in particular to a detection device for hydrogen chloride content in a gas phase of a hydrogenation device and a gas circuit system.
Background
Hydrogenation is an important link in the petroleum processing process, has important significance for improving the processing depth of crude oil, improving the quality of oil products, improving the yield of light oil and the like, and especially has more importance for continuously increasing the market demand on high-quality middle distillate oil along with the gradual deterioration of the crude oil. In the reaction effluent system of a hydrogenation unit, the problem of corrosion of equipment such as a heat exchanger, an air cooler and the like caused by deposition of ammonium salt is always a 'stubborn disease' which troubles the hydrogenation unit, particularly NH4A salt of Cl. Due to the chloride contained in the fresh hydrogen (make-up hydrogen) and the hydrogenated raw oil, the gas phase of the reaction effluent contains trace HCl, while NH in the gas phase of the reaction effluent3And HCl can form solid NH4Cl salt, NH4Cl salt has strong hygroscopicity, and trace amount of liquid water, NH, can appear once the temperature of reaction effluent is slightly lower than the dew point temperature of water4The Cl salt can form an extremely low pH value environment under the condition of moist scale salt, and serious corrosion is caused to equipment. Therefore, it is necessary to detect the trace HCl content in the gas path system of the hydrogenation apparatus, i.e., fresh hydrogen, recycle hydrogen, and the gas phase of the hydrogenation reaction effluent.
The detection of trace HCl content in the gas circuit system of the hydrogenation device has no fixed standard, so most refineries have less analysis on the trace HCl content, and the existing detection devices are fewer. The patent with the application number of 201910639640.X discloses a method and a device for detecting trace hydrogen chloride in a gas phase of a hydrogen device, but the application range is narrow, and the detection result is inaccurate.
In view of this, the present application is specifically made.
Disclosure of Invention
The invention aims to provide a device for detecting the content of hydrogen chloride in a gas phase of a hydrogenation device, which can realize the adjustment of the pressure and the flow of gas in a detection pipeline, thereby having wider detection range and higher applicability. In addition, this application can effectively avoid the steam in the gas to condense before getting into the absorption vessel, and HCl in the gas can be totally in the absorption vessel condensation, and the testing result is more accurate.
The invention aims to provide a gas circuit system which can effectively detect HCl in the gas circuit system so as to provide certain guidance suggestion for a hydrogenation link.
Embodiments of the invention may be implemented as follows:
in a first aspect, the invention provides a device for detecting the content of hydrogen chloride in a gas phase of a hydrogenation device, which comprises a detection pipeline, an absorption container and a cooling container, wherein the detection pipeline is used for being communicated with a sampling pipeline preset in a gas pipeline of the hydrogenation device, the absorption container is used for containing alkaline absorption liquid, the cooling container is used for condensing hydrogen chloride entering the absorption container, a pressure reducing valve, a pressure gauge and a flow regulating valve are sequentially arranged on the detection pipeline, the tail end of the detection pipeline is communicated with the absorption container, the absorption container is arranged in the cooling container, and heat insulation layers are sleeved on the detection pipeline and the outer side of the cooling container.
In an alternative embodiment, the absorption container comprises a first absorption container and a second absorption container which are connected in series, the first absorption container is communicated with the tail end of the detection pipeline, and a vortex shedding flowmeter is connected to the rear end of the second absorption container.
In an optional embodiment, a sealing cover is arranged in the cooling container, the sealing cover is provided with a round hole, and the upper part of the absorption container penetrates through the round hole.
In an optional embodiment, a partition plate for placing the absorption container is arranged in the cooling container, a groove is arranged on the partition plate, and the bottom of the absorption container is placed in the groove.
In an optional embodiment, the pressure reducing valve comprises a first pressure reducing valve and a second pressure reducing valve, the pressure gauge comprises a first pressure gauge and a second pressure gauge, the first pressure gauge is arranged between the first pressure reducing valve and the second pressure reducing valve, and the second pressure gauge is arranged at the rear side of the second pressure reducing valve.
In an optional embodiment, the flow regulating valve includes a first flow regulating valve, a second flow regulating valve and a third flow regulating valve, the first flow regulating valve and the second flow regulating valve are sequentially installed at the rear side of the second pressure gauge, the third flow regulating valve and the rotameter are sequentially installed between the first flow regulating valve and the second flow regulating valve in a direction perpendicular to the detection pipeline, the rear side of the rotameter is empty, and the rear side of the second flow regulating valve is communicated with the absorption container.
In an alternative embodiment, the detection pipeline is made of teflon.
In an optional embodiment, the apparatus for detecting the content of hydrogen chloride in the gas phase of the hydrogenation apparatus further comprises a movable platform, and the detection pipeline, the absorption container and the cooling container are all mounted on the movable platform.
In an alternative embodiment, the concentration of the alkaline absorption solution is from 0.1mol/L to 1 mol/L.
In a second aspect, the present invention provides a gas path system, which includes a sampling pipeline and a device for detecting the content of hydrogen chloride in the gas phase of a hydrogenation apparatus according to any one of the foregoing embodiments, wherein the detection pipeline of the device for detecting the content of hydrogen chloride in the gas phase of a hydrogenation apparatus is communicated with the sampling pipeline, and a sampling flow regulating valve is disposed on the sampling pipeline.
The beneficial effects of the embodiment of the invention include, for example:
according to the detection device for the content of hydrogen chloride in the gas phase of the hydrogenation device, provided by the embodiment of the invention, the pressure and the flow of the gas in the detection pipeline can be adjusted by arranging the pressure reducing valve, the pressure gauge and the flow regulating valve on the detection pipeline, so that the detection device for the content of hydrogen chloride in the gas phase of the hydrogenation device has the advantages of wider detection range and higher applicability, can be used for detecting the content of HCl in a low-pressure gas circuit system of the hydrogenation device, and can also be used for detecting a medium-pressure gas circuit system and a high-pressure gas circuit system. In addition, in this application, the whole heat preservation that keeps warm before getting into the absorption vessel is gone on to the detection pipeline, can effectively avoid the steam in the gas to condense before getting into the absorption vessel, causes the inaccurate condition of testing result to take place. And the last heat preservation that sets up of cooling container can guarantee when detection ring border temperature is higher, and the ice-cube in the cooling container still can keep cold for a long time, effectively avoids appearing HCl in the gas and can not be totally in the absorption vessel condensation, causes HCl to absorb inadequately, and the condition that the testing result is lower takes place. The gas circuit system provided by the embodiment can effectively detect HCl in the gas circuit system, and the detection result is accurate.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained according to the drawings without inventive efforts.
Fig. 1 is a schematic structural diagram of a device for detecting the content of hydrogen chloride in a gas phase of a hydrogenation device provided in an embodiment of the present application;
FIG. 2 is a schematic structural diagram of a separator of a device for detecting the content of hydrogen chloride in a gas phase of a hydrogenation device provided in an embodiment of the present application;
fig. 3 is a schematic structural diagram of a sealing cover of a detection device for detecting the content of hydrogen chloride in a gas phase of a hydrogenation device provided in an embodiment of the present application;
fig. 4 is a schematic structural diagram of a gas circuit system in a hydrogenation apparatus provided in the embodiment of the present application in cooperation with a detection apparatus for detecting a hydrogen chloride content in a gas phase of the hydrogenation apparatus.
Icon: 100-a device for detecting the content of hydrogen chloride in the gas phase of a hydrogenation device;
110-detecting the pipeline; 111-a pressure relief valve; 1111-a first pressure reducing valve; 1112-a second pressure relief valve; 112-pressure gauge; 1121-first pressure gauge; 1122-a second pressure gauge; 113-a flow regulating valve; 1131 — first flow regulating valve; 1132 — a second flow regulating valve; 1133-third flow regulating valve; 114-a rotameter;
120-an absorption vessel; 121-a first absorption vessel; 122-a second absorption vessel; 123-alkaline absorption liquid;
130-a cooling vessel; 131-a separator; 132-a groove; 133-a sealing cover; 134-round hole;
140-a movable platform;
200-a gas path system; 201-a sampling pipe; 202-sample flow regulating valve.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all, embodiments of the present invention. The components of embodiments of the present invention generally described and illustrated in the figures herein may be arranged and designed in a wide variety of different configurations.
Thus, the following detailed description of the embodiments of the present invention, presented in the figures, is not intended to limit the scope of the invention, as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
It should be noted that: like reference numbers and letters refer to like items in the following figures, and thus, once an item is defined in one figure, it need not be further defined and explained in subsequent figures.
In the description of the present invention, it should be noted that if the terms "upper", "lower", "inside", "outside", etc. indicate an orientation or a positional relationship based on that shown in the drawings or that the product of the present invention is used as it is, this is only for convenience of description and simplification of the description, and it does not indicate or imply that the device or the element referred to must have a specific orientation, be constructed in a specific orientation, and be operated, and thus should not be construed as limiting the present invention.
Furthermore, the appearances of the terms "first," "second," and the like, if any, are used solely to distinguish one from another and are not to be construed as indicating or implying relative importance.
It should be noted that the features of the embodiments of the present invention may be combined with each other without conflict.
Examples
Referring to fig. 1, the present embodiment provides a device 100 for detecting the content of hydrogen chloride in a gas phase of a hydrogenation apparatus, which includes a detection pipe 110, an absorption container 120, a cooling container 130, and a movable platform 140, wherein the end of the detection pipe 110 is communicated with the absorption container 120, the absorption container 120 is disposed in the cooling container 130, and the detection pipe 110, the absorption container 120, and the cooling container 130 are all mounted on the movable platform 140.
The detection pipeline 110 is used for being communicated with a sampling pipeline 201 preset in a gas pipeline of the hydrogenation device, so that gas in the gas pipeline of the hydrogenation device is led out to the detection pipeline 110 for subsequent detection.
Specifically, the detection pipe 110 is provided with a pressure reducing valve 111, a pressure gauge 112, and a flow rate adjusting valve 113 in this order. The pressure reducing valve 111 is used for reducing the pressure of the gas in the detection pipe 110, the pressure gauge 112 is used for detecting the pressure condition after the pressure reduction, and the flow regulating valve 113 is used for regulating the flow of the gas.
In this application, the relief valve 111 is two, specifically includes first relief valve 1111 and second relief valve 1112, and is the same, and manometer 112 also is two, specifically includes first manometer 1121 and second manometer 1122, and first manometer 1121 sets up between first relief valve 1111 and second relief valve 1112, and second manometer 1122 sets up in the rear side of second relief valve 1112. Through setting up two relief pressure valves 111 and two manometer 112 in this application, can realize carrying out slowly many times to the pressure of detecting the gas in the pipeline 110 and adjust, under the complete condition is not adjusted to first relief pressure valve 1111 simultaneously, can also utilize second relief pressure valve 1112 to continue to adjust, and gas pressure's accuracy has been guaranteed to two manometer 112.
Set up relief pressure valve 111 in this application, not only can detect the HCl content in the gas circuit system 200 of the low pressure of hydrogenation unit, can also detect middle, high pressure gas circuit system 200, detection range in hydrogenation unit is wider, the suitability is higher.
In this application, the flow control valves 113 are three, and specifically include a first flow control valve 1131, a second flow control valve 1132, and a third flow control valve 1133, wherein the first flow control valve 1131 and the second flow control valve 1132 are sequentially installed on the rear side of the second pressure gauge 1122, the third flow control valve 1133 and the rotameter 114 are sequentially installed between the first flow control valve 1131 and the second flow control valve 1132 in the direction perpendicular to the detection pipeline 110, the rear side of the rotameter 114 is empty, and the rear side of the second flow control valve 1132 is communicated with the absorption container 120. In the present application, the first flow rate adjustment valve 1131 performs a first flow rate adjustment, and then, the third flow rate adjustment valve 1133 performs a second flow rate adjustment to make the flow rate constant, and the flow rate is read by the rotameter 114 to be fixed at 0.1L/min to 2L/min. When the pressure and flow regulation is completed, the third flow regulating valve 1133 is closed, the second flow regulating valve 1132 is opened, and the sampling is started.
The detection pipeline 110 is made of polytetrafluoroethylene, and the polytetrafluoroethylene is high in acid and alkali corrosion resistance, so that pipeline corrosion is avoided, the purity of collected gas is high, and the measurement result is accurate. The heat preservation layer is sleeved on the outer side of the detection pipeline 110, and the heat preservation layer can effectively prevent water vapor in gas from condensing before entering the absorption container 120, so that the situation that the detection result is inaccurate occurs.
The absorption vessel 120 is for containing an alkaline absorbent liquid 123. In the present application, the absorption container 120 includes a first absorption container 121 and a second absorption container 122 connected in series, the first absorption container 121 is communicated with the end of the detection pipe 110, and a vortex shedding flowmeter is connected to the rear end of the second absorption container 122.
The gas discharged from the detection pipeline 110 enters the first absorption container 121 for absorption, and enters the second absorption container 122 again for secondary absorption after complete absorption, and the HCl in the gas can be completely absorbed and condensed by the first absorption container 121 and the second absorption container 122 which are connected in series in the application.
This applicationThe concentration of the alkaline absorption liquid 123 is determined according to NH in acidic water of a reaction effluent separation unit of the hydrogenation device4Preparing alkaline absorption liquid 123(NaOH or KOH solution) according to the HS concentration or the Kp coefficient of ammonium bisulfide, wherein the basic absorption liquid 123 is prepared according to the principle that the basic absorption liquid 123 absorbing the acid gas is still alkaline after the detection work is finished. In the present application, the concentration of the alkaline absorbent 123 is in the range of 0.1mol/L to 1 mol/L. When NH is present4When the concentration of HS is not more than 4 wt.% or the Kp coefficient of ammonium bisulfide is not more than 0.3, the concentration of the alkaline absorption liquid 123 is 0.1-0.5 mol/L; when NH is present4When the concentration of HS exceeds 4 wt.% or the Kp coefficient of ammonium bisulfide exceeds 0.3, the concentration of the alkaline absorption liquid 123 is 0.5-1 mol/L. The first absorption vessel 121 and the second absorption vessel 122 each contain the alkaline absorbent 123 in an amount of 50 mL.
The cooling vessel 130 is used to condense the hydrogen chloride entering the absorber vessel 120. In order to facilitate stable placement of the absorption vessel 120 within the cooling vessel 130. Referring to fig. 2 and 3, in the present application, a partition 131 for placing the absorption container 120 is disposed in the cooling container 130, and a sealing cover 133 is disposed in the cooling container 130, the sealing cover 133 is located above the partition 131, a groove 132 is disposed on the partition 131, the bottom of the absorption container 120 is placed in the groove 132, a circular hole 134 is formed in the sealing cover 133, and the upper portion of the absorption container 120 is inserted into the circular hole 134. In the present application, the cooling container 130 and the sealing cover 133 are both provided with insulating layers. Make absorption vessel 120 place the position through setting up of baffle 131 fixed, the setting of sealed lid 133 not only can further inject absorption vessel 120's the position of placing simultaneously, can also effectively carry out cold insulation to the ice-cube in cooling vessel 130 simultaneously, effectively avoid under the higher circumstances of detection ring border temperature, the ice-cube in cooling vessel 130 melts, lead to HCl in the gas can not be totally condensed in absorption vessel 120, cause HCl to absorb inadequately, the condition that the testing result is lower takes place.
The movable platform 140 is used for placing the detection pipeline 110, the absorption container 120 and the cooling container 130, so that the whole detection device is convenient to move and disassemble and simple to operate.
The working process of the detection device 100 for the hydrogen chloride content in the gas phase of the hydrogenation device provided by the application is as follows:
s1, before detection, the valves of the detection device are checked to be in a closed state.
S2, separating NH in acidic water according to reaction effluent of hydrogenation unit4Preparing alkaline absorption liquid 123(NaOH or KOH solution) according to the HS concentration or the Kp coefficient of ammonium bisulfide, wherein the basic absorption liquid 123 is prepared according to the principle that the basic absorption liquid 123 absorbing the acid gas is still alkaline after the detection work is finished. Generally, the concentration of the alkaline absorbent 123 is in the range of 0.1mol/L to 1 mol/L. When NH is present4When the concentration of HS is not more than 4 wt.% or the Kp coefficient of ammonium bisulfide is not more than 0.3, the concentration of the alkaline absorption liquid 123 is 0.1-0.5 mol/L; when NH is present4When the concentration of HS exceeds 4 wt.% or the Kp coefficient of ammonium bisulfide exceeds 0.3, the concentration of the alkaline absorption liquid 123 is 0.5-1 mol/L.
S3, 50mL of the prepared alkaline absorbent 123 was transferred to the first absorption vessel 121 and the second absorption vessel 122, respectively.
And S4, adjusting the gas pressure and the gas flow of the detection device. If the gas pressure in the gas circuit system 200 to be detected is high, such as hot high-pressure gas, cold high-pressure gas, circulating hydrogen, etc., the five valves, i.e., the sampling port flow regulating valve 113, the first reducing valve 1111, the second reducing valve 1112, the first flow regulating valve 1131, and the third flow regulating valve 1133, are opened and slowly adjusted, so that the gas pressure and flow of the detection device are constant. The final pressure is read by a second pressure gauge 1122 and the gas flow is read by rotameter 114. Generally, the flow rate is fixed at 0.1L/min to 2L/min. If the gas pressure in the gas circuit system 200 to be measured is low, the pressure reduction operation may not be performed.
And S5, after the gas pressure and flow of the detection device are adjusted, closing the first flow adjusting valve 1131, opening the second flow adjusting valve 1132, and starting sampling, wherein the sampling time is 30-60 min. And in the sampling process, reading the instantaneous flow and the accumulated flow of the vortex shedding flowmeter at equal time intervals. And after sampling is finished, reading the accumulated flow of the vortex shedding flowmeter, wherein the deviation of the instantaneous flow before and after sampling is not more than 3%.
S6, closing all valves of the detection device, sealing the two absorption containers 120 for low-temperature storage, performing ion chromatography analysis on the content of chloride ions in the absorption liquid as soon as possible, and calculating the content of trace HCl in the gas.
The application provides a detection device 100 of hydrogen chloride content in hydrogenation device gaseous phase, through set up relief pressure valve 111 on detecting pipeline 110, manometer 112 and flow control valve 113, can realize adjusting the pressure and the flow of gas in detecting pipeline 110, thereby make the detection range of detection device 100 of hydrogen chloride content in the hydrogenation device gaseous phase of this application wider, the suitability is higher, not only can detect the HCl content in the gas circuit system 200 of low pressure of hydrogenation device, can also the centering, highly compressed gas circuit system 200 detects. In addition, in this application, the whole journey of detection pipeline 110 before getting into absorption vessel 120 keeps warm, can effectively avoid the steam in the gas to condense before getting into absorption vessel 120, causes the inaccurate condition of testing result to take place. And the heat preservation that sets up on cooling container 130 can guarantee when detection ambient temperature is higher, and the ice-cube in cooling container 130 still can keep cold for a long time, effectively avoids appearing HCl in the gas and can not be totally condensed in absorption vessel 120, causes HCl to absorb inadequately, and the condition that the testing result is lower takes place. The detection pipeline 110 is made of polytetrafluoroethylene, is high in acid and alkali corrosion resistance, avoids pipeline corrosion, and enables the purity of collected gas to be high and the measurement result to be accurate. In addition, the detection device of the invention is integrally fixed on the movable platform 140, and has the advantages of convenient movement, disassembly and assembly, simple operation and convenient carrying.
In addition, referring to fig. 4, the present invention further provides a gas path system 200, which includes a sampling pipe 201 and a detection device 100 for detecting the content of hydrogen chloride in the gas phase of the hydrogenation apparatus, wherein the detection pipe 110 of the detection device 100 for detecting the content of hydrogen chloride in the gas phase of the hydrogenation apparatus is communicated with the sampling pipe 201, and the sampling pipe 201 is provided with a sampling flow regulating valve 202.
In summary, according to the detection device 100 for detecting the content of hydrogen chloride in the gas phase of the hydrogenation device provided in the embodiment of the present invention, the pressure reducing valve 111, the pressure gauge 112, and the flow regulating valve 113 are disposed on the detection pipeline 110, so that the pressure and the flow of the gas in the detection pipeline 110 can be regulated, and thus the detection device 100 for detecting the content of hydrogen chloride in the gas phase of the hydrogenation device of the present application has a wider detection range and higher applicability, and can not only detect the content of HCl in the low-pressure gas circuit system 200 of the hydrogenation device, but also detect the medium-pressure and high-pressure gas circuit systems 200. In addition, in this application, the whole journey of detection pipeline 110 before getting into absorption vessel 120 keeps warm, can effectively avoid the steam in the gas to condense before getting into absorption vessel 120, causes the inaccurate condition of testing result to take place. And the heat preservation that sets up on cooling container 130 can guarantee when detection ambient temperature is higher, and the ice-cube in cooling container 130 still can keep cold for a long time, effectively avoids appearing HCl in the gas and can not be totally condensed in absorption vessel 120, causes HCl to absorb inadequately, and the condition that the testing result is lower takes place. The gas circuit system 200 provided by this embodiment can effectively detect HCl in the gas circuit system 200, and the detection result is accurate.
The above description is only for the specific embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are included in the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the appended claims.
Claims (10)
1. The utility model provides a detection apparatus for hydrogen chloride content in hydrogenation device gas phase, its characterized in that, including be used for with the detection pipeline of the gas circuit pipeline preset of hydrogenation device intercommunication, be used for holding the absorption vessel of alkaline absorption liquid and be used for to getting into hydrogen chloride carries out the cooling container of condensation in the absorption vessel, pressure reducing valve, manometer and flow control valve have set gradually on the detection pipeline, the end of detection pipeline with the absorption vessel intercommunication, the absorption vessel set up in the cooling container, the detection pipeline with the cooling container outside all is equipped with the heat preservation.
2. The device for detecting the content of hydrogen chloride in the gas phase of a hydrogenation unit according to claim 1, wherein the absorption container comprises a first absorption container and a second absorption container which are connected in series, the first absorption container is communicated with the tail end of the detection pipeline, and a vortex shedding flowmeter is connected to the rear end of the second absorption container.
3. The apparatus for detecting the content of hydrogen chloride in a gas phase of a hydrogenation apparatus according to claim 1, wherein a sealing cover is disposed in the cooling container, the sealing cover is provided with a circular hole, and the upper portion of the absorption container is inserted into the circular hole.
4. The device for detecting the content of hydrogen chloride in the gas phase of the hydrogenation device according to claim 3, wherein a partition plate for placing the absorption container is arranged in the middle of the cooling container, a groove is formed in the partition plate, and the bottom of the absorption container is placed in the groove.
5. The apparatus according to claim 1, wherein the pressure reducing valve comprises a first pressure reducing valve and a second pressure reducing valve, the pressure gauge comprises a first pressure gauge and a second pressure gauge, the first pressure gauge is disposed between the first pressure reducing valve and the second pressure reducing valve, and the second pressure gauge is disposed at a rear side of the second pressure reducing valve.
6. The hydrogenation apparatus according to claim 5, wherein the flow control valve comprises a first flow control valve, a second flow control valve and a third flow control valve, the first flow control valve and the second flow control valve are sequentially mounted on the rear side of the second pressure gauge, the third flow control valve and a rotameter are sequentially mounted between the first flow control valve and the second flow control valve in a direction perpendicular to the detection pipeline, the rear side of the rotameter is empty, and the rear side of the second flow control valve is communicated with the absorption container.
7. The device for detecting the content of hydrogen chloride in the gas phase of the hydrogenation device according to any one of claims 1 to 6, wherein the detection pipeline is made of polytetrafluoroethylene.
8. The apparatus for detecting the content of hydrogen chloride in the gas phase of a hydrogenation unit as claimed in any one of claims 1 to 6, wherein the apparatus for detecting the content of hydrogen chloride in the gas phase of a hydrogenation unit further comprises a movable platform, and the detection pipeline, the absorption vessel and the cooling vessel are all mounted on the movable platform.
9. The device for detecting the content of hydrogen chloride in the gas phase of the hydrogenation device according to any one of claims 1 to 6, wherein the concentration of the alkaline absorption liquid is 0.1mol/L to 1 mol/L.
10. A gas path system, characterized in that it comprises a sampling pipeline and a device for detecting the content of hydrogen chloride in the gas phase of a hydrogenation device according to any one of claims 1 to 9, the detection pipeline of the device for detecting the content of hydrogen chloride in the gas phase of a hydrogenation device is communicated with the sampling pipeline, and the sampling pipeline is provided with a sampling flow regulating valve.
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