CN111781024A - Tandem type negative pressure sampling analysis system and method - Google Patents
Tandem type negative pressure sampling analysis system and method Download PDFInfo
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- 238000005070 sampling Methods 0.000 title claims abstract description 195
- 238000004458 analytical method Methods 0.000 title claims abstract description 85
- 238000000034 method Methods 0.000 title claims abstract description 24
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 207
- 239000007789 gas Substances 0.000 claims abstract description 129
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 103
- 239000007788 liquid Substances 0.000 claims abstract description 21
- 238000010926 purge Methods 0.000 claims abstract description 13
- 230000008569 process Effects 0.000 claims abstract description 9
- 239000000463 material Substances 0.000 claims description 28
- 238000011144 upstream manufacturing Methods 0.000 claims description 17
- 238000012544 monitoring process Methods 0.000 claims description 11
- 238000010574 gas phase reaction Methods 0.000 claims description 9
- 238000004868 gas analysis Methods 0.000 claims description 8
- 238000005086 pumping Methods 0.000 claims description 7
- 230000009471 action Effects 0.000 claims description 4
- 230000001502 supplementing effect Effects 0.000 claims 1
- 238000006243 chemical reaction Methods 0.000 abstract description 32
- 238000004321 preservation Methods 0.000 abstract description 6
- YNQLUTRBYVCPMQ-UHFFFAOYSA-N Ethylbenzene Chemical compound CCC1=CC=CC=C1 YNQLUTRBYVCPMQ-UHFFFAOYSA-N 0.000 description 30
- 239000012071 phase Substances 0.000 description 28
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 16
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 12
- 238000006356 dehydrogenation reaction Methods 0.000 description 11
- 239000007791 liquid phase Substances 0.000 description 5
- 230000001276 controlling effect Effects 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 230000001105 regulatory effect Effects 0.000 description 4
- 230000005494 condensation Effects 0.000 description 3
- 238000009833 condensation Methods 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 238000013461 design Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- XECAHXYUAAWDEL-UHFFFAOYSA-N acrylonitrile butadiene styrene Chemical compound C=CC=C.C=CC#N.C=CC1=CC=CC=C1 XECAHXYUAAWDEL-UHFFFAOYSA-N 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- 238000006073 displacement reaction Methods 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- 239000012495 reaction gas Substances 0.000 description 2
- 239000004793 Polystyrene Substances 0.000 description 1
- GOOHAUXETOMSMM-UHFFFAOYSA-N Propylene oxide Chemical compound CC1CO1 GOOHAUXETOMSMM-UHFFFAOYSA-N 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000013064 chemical raw material Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 229920006351 engineering plastic Polymers 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 230000002452 interceptive effect Effects 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 229920002223 polystyrene Polymers 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000012808 vapor phase Substances 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
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/02—Devices for withdrawing samples
- G01N1/10—Devices for withdrawing samples in the liquid or fluent state
- G01N1/14—Suction devices, e.g. pumps; Ejector devices
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/02—Devices for withdrawing samples
- G01N1/10—Devices for withdrawing samples in the liquid or fluent state
- G01N1/14—Suction devices, e.g. pumps; Ejector devices
- G01N2001/1418—Depression, aspiration
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- Chemical & Material Sciences (AREA)
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- General Health & Medical Sciences (AREA)
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Abstract
The invention provides a tandem negative pressure sampling analysis system and a method, which comprises a sampling pipeline, an oil bath device, a gas phase analysis component, a buffer tank, a vacuum pump, a flow control component, a pressure control component and a nitrogen purging component, wherein the gas phase analysis component, the buffer tank and the vacuum pump are sequentially connected in series through pipelines to form a tandem sampling analysis structure, all pipelines in front of the buffer tank are subjected to heat preservation or electric tracing, a sample is kept in a gas phase state before entering a gas chromatograph, gas-liquid two phases are avoided, and the sample is pumped into the gas chromatograph through the vacuum pump, so that the online sampling and analysis of a negative pressure system are realized. And by adopting a gas phase sampling mode, the sample replacement time in a sampling pipeline is short, the sampling quality is low, and the interference of the sampling process on a reaction system can be reduced. The entire sampling and analysis system is integrated into the same control system. Automatic valves and instruments are arranged at necessary positions, so that automatic sampling and sample introduction are realized.
Description
Technical Field
The invention relates to the technical field of negative pressure sampling analysis, in particular to a serial negative pressure sampling analysis system and a serial negative pressure sampling analysis method.
Background
In the field of petrochemical industry, some reactions are carried out in a negative pressure environment, and the reaction in a negative pressure system needs to maintain the whole reaction process in a negative pressure state so as to ensure the normal operation of the reaction. Styrene is an important chemical raw material and can be used for producing engineering plastic materials such as polystyrene, acrylonitrile-styrene-butadiene (ABS) and the like. At present, the production method of styrene mainly comprises an ethylbenzene dehydrogenation method and a styrene/propylene oxide coproduction method. Wherein, the ethylbenzene dehydrogenation method is dominant, and the proportion is over 90 percent. The main reactions in the dehydrogenation of ethylbenzene are: c6H5C2H5＝C6H5-C2H3+H2。
As shown in fig. 2, industrially, an ethylbenzene dehydrogenation reactor operates under high temperature, negative pressure, adiabatic conditions. The reaction temperature is about 580-630 ℃, and the lowest reaction pressure can reach negative pressure of 30 kPa. Industrially, two adiabatic reactors, a first reactor 1 and a second reactor 2, are generally arranged in series. Since the reaction is endothermic, the temperature of the reaction mass after it has been reacted in the first reactor 1 is generally reduced from about 620 ℃ to below 600 ℃. Thereafter, the stream is heated to about 620 ℃ and then fed to the second reactor 2 to continue the reaction.
In an industrial installation for ethylbenzene dehydrogenation, in order to evaluate the performance of the catalyst in time and at the same time provide a reference for the operation of the downstream separation unit, it is necessary to take samples at the two reactor inlets (a and B) and at the two reactor outlets (C and D), for a total of 4 sampling points (A, B, C and D), and to carry out a composition analysis thereof. For the ethylbenzene dehydrogenation pilot plant, in order to obtain complete data in the pilot process for the design of industrial scale reactors and the design of process flows, the information of samples of the 4 sampling points is also required to be obtained.
For the above sample collection of 4 sampling points, the prior art is mainly as follows: a condenser is arranged at the sampling port to cool the sample from a gas state to a liquid and gas mixed state. A sampler is arranged downstream of the condenser. After the sampler is vacuumized, the valve is opened, so that the liquid can flow into the sampling tank, and then the liquid phase analysis is carried out. Chinese utility model patent No. CN201476995U discloses such a vacuum sampling system.
The main defects of the prior art are as follows: 1) gas phase samples could not be analyzed. By adopting the existing method, a sample can be separated into a gas phase and a liquid phase after being cooled by a condenser. A sample of the liquid phase is taken through the lower part of the sampling flask. But samples in the gas phase cannot be analyzed. 2) Interfering with the reaction system. When a sample is collected by this method, a part of the material is diverted from the reaction system by the sampling line, which causes a deviation in the feed flow rate into the reaction bed at the time of sampling.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: in order to overcome the defects in the prior art, the invention provides a serial negative pressure sampling analysis system and a serial negative pressure sampling analysis method, which can enable a sample to be collected in a gas phase state and then sent to a detection instrument for analysis so as to obtain the composition of the sample and further obtain the complete composition information of the sample; because the sample is a gas phase, the sampling quality is very small, and the sampling time is short, so that the interference of the sampling process to the reaction system is small; and a full-automatic sampling and analyzing mode is adopted, so that the labor is saved, the efficiency is improved, and the operation error rate is reduced.
In order to clearly understand the technical scheme of the present invention, the following terms are explained, in the present invention, negative pressure and positive pressure are relative to 1 standard atmospheric pressure, negative pressure refers to a pressure state of less than 1 standard atmospheric pressure, and positive pressure refers to a pressure state of more than 1 standard atmospheric pressure.
The technical scheme adopted for solving the technical problems is as follows: a serial negative pressure sampling analysis system comprises a sampling pipeline, an oil bath device, a gas phase analysis component, a buffer tank, a vacuum pump, a flow control component and a pressure control component, wherein one end of the sampling pipeline is connected to a sampling point of a reactor and used for sampling and inputting gas phase reaction materials, the other end of the sampling pipeline is connected to one end of a sampling pipeline control valve after passing through the oil bath device, the other end of the sampling pipeline control valve is connected to a gas phase inlet and outlet end of the gas phase analysis component through a pipeline, an automatic two-way valve is adopted as a preferred sampling pipeline control valve, the flow control component is arranged on the pipeline between the sampling pipeline control valve and the gas phase analysis component, the other gas phase inlet and outlet end of the gas phase analysis component is connected to the buffer tank through a pipeline, one outlet of the buffer tank is connected to the vacuum pump through a pipeline, one, the pressure control assembly is used for monitoring the pressure in the upstream and downstream pipelines of the gas phase analysis assembly and the pressure in the buffer tank, and controlling the air inflow of the first nitrogen inlet according to the monitored pressure; the gas phase analysis assembly, the buffer tank and the vacuum pump are sequentially connected in series through pipelines to form a serial-type sampling analysis structure.
Further, in order to realize the analysis of the components of the reaction materials, the gas analysis component comprises a gas chromatograph, a first automatic three-way valve and a second automatic three-way valve, the gas chromatograph is connected in series on a pipeline between the buffer tank and the flow control component through the first automatic three-way valve and the second automatic three-way valve, and two ends of the gas chromatograph are also connected with a branch pipeline in parallel through the first automatic three-way valve and the second automatic three-way valve.
Further, in order to control the flow in the sampling pipeline within a smaller flow range, the flow control assembly comprises a flow control valve and a flow display controller, wherein the flow control valve is preferably an automatic two-way valve, the flow control valve is arranged on the pipeline at the upstream of the gas phase analysis assembly, the flow display controller is in signal connection with a control end of the flow control valve, and the flow display controller is used for setting and displaying the flow and monitoring the flow in the sampling pipeline and adjusting the opening of the flow control valve according to the set flow and the monitored flow in the pipeline. When the flow display controller sets a smaller flow, the opening of the flow control valve is in a smaller state, so that the quantity of the reaction materials collected in the control pipeline is in a smaller quantity, and the influence on the reaction materials in the main pipeline and the reaction environment in the reactor is avoided.
Further, in order to avoid unstable reaction state in the reactor caused by large pressure difference, the pressure control assembly comprises a pressure display controller and a first nitrogen inlet valve, preferably, the first nitrogen inlet valve adopts an automatic two-way valve, the first nitrogen inlet valve is connected in series on a pipeline between the buffer tank and the first nitrogen inlet, the pressure display controller is in signal connection with a control end of the first nitrogen inlet valve, the pressure display controller is used for setting and displaying pressure and monitoring the pressure in the buffer tank, and the opening degree of the first nitrogen inlet valve is adjusted according to the set pressure and the monitored pressure in the buffer tank. The pressure control assembly enables the pressure in the sampling analysis system and the pressure in the reactor and the main pipeline thereof to generate a smaller pressure difference, so that the sampling gas can be ensured to enter the sampling analysis system under the action of the pressure difference, and the buffer tank can also prevent suck-back and protect the vacuum pump.
Furthermore, a manual two-way valve is respectively arranged on the pipelines at the upstream and downstream of the first nitrogen inlet valve, wherein the manual two-way valve is used for directly cutting off the airflow of the first nitrogen inlet, and the first nitrogen inlet valve is used for regulating and controlling the flow of nitrogen; the main pipeline formed by the first nitrogen inlet valve and the manual two-way valve is also connected with a branch pipeline in parallel, and the branch pipeline is provided with a manual two-way valve as a branch air inlet valve. When the valve on the main pipeline breaks down and can not be filled with nitrogen, the branch inlet valve on the branch pipeline is opened to fill nitrogen.
And pipelines in front of the buffer tank are provided with heat preservation or heating devices. The sampling gas is kept in a heat preservation or electric heat tracing state all the time, the sampling material is kept in a gas state all the time, a constant-temperature oil bath is adopted as an optimal oil bath device, and the constant-temperature oil bath has the functions of temperature display and temperature control.
Furthermore, in order to facilitate on-off control of air flow in the pipeline, a vacuumizing control valve is arranged on the pipeline between the buffer tank and the vacuum pump, a liquid discharge pipe is arranged at the bottom of the buffer tank, and a liquid discharge control valve is arranged on the liquid discharge pipe. An automatic two-way valve is adopted as a preferred vacuumizing control valve, and a manual two-way valve is adopted as a liquid discharge control valve.
Further, in order to enable the system to simultaneously meet the gas composition analysis of a plurality of sampling points, the system further comprises a nitrogen purging assembly arranged at the upstream of the flow control assembly, wherein the nitrogen purging assembly comprises a second nitrogen inlet and a second nitrogen inlet valve, and the second nitrogen inlet is connected to a main pipeline at the upstream of the flow control assembly through a pipeline through the second nitrogen inlet valve. The second nitrogen inlet valve is preferably an automatic two-way valve. And the sampling gas at the previous sampling point in the system is exhausted through the nitrogen purging assembly, so that multi-point continuous sampling analysis is facilitated.
Further, in order to avoid the discharged gas from polluting the environment, the device also comprises an ice bath device, wherein the buffer tank is arranged in the ice bath device, and the temperature range of the ice bath is 5-15 ℃. The buffer tank is in ice bath, so that heavier components such as benzene, ethylbenzene, styrene and the like are condensed into liquid without being discharged.
A series connection type vacuum sampling analysis method comprises the vacuum sampling analysis system, and the method is mainly divided into five stages, namely a parameter setting stage, a pressure adjusting stage, a pipeline emptying stage, a sampling analysis stage and a nitrogen purging stage, and the steps and the functions of each stage are explained in detail below.
The parameter setting stage comprises the following steps:
step S0: in order to realize automatic sampling analysis, the control system sets the operation time of automatic sampling and analysis, and the control system controls the sampling analysis system to automatically execute sampling according to the set time.
The pressure adjusting phase comprises the following steps:
s1: adjusting the on-off state of a valve in the system to enable the sampling pipeline control valve, the second nitrogen inlet valve, the flow control valve, the vacuumizing control valve and the liquid discharge control valve to be in a closed state; a valve on a branch pipeline between the first nitrogen inlet and the buffer tank is in a closed state; and adjusting the directions of the first automatic three-way valve and the second automatic three-way valve in the gas analysis assembly to enable the gas chromatograph to be in a state of not being connected with a pipeline between the flow control valve and the buffer tank.
S2: the vacuum pump and the vacuumizing control valve are opened to vacuumize, meanwhile, the target pressure value of the pressure display controller is set to be smaller than the pressure value at the inlet of the upstream reactor, the target pressure is generally set to be about 90% of the material pressure at the inlet of the reactor, namely, about 10% of the material pressure at the inlet of the reactor, and preferably, the target pressure can be reduced by 5kPa, for example: the material pressure at the inlet of the reactor is 60kPa, the target pressure is 55kPa, and the pressure difference can be adjusted according to the material pressure at the inlet of the reactor. And nitrogen is introduced into the buffer tank through a main line of the first nitrogen inlet, the pressure display controller monitors the pressure in the buffer tank, and the opening degree of the first nitrogen inlet valve is adjusted according to the monitored pressure and the target pressure value, so that the pressure in the buffer tank reaches and maintains the target pressure value.
S3: and when the pressure in the buffer tank reaches the target pressure value, opening the flow control valve to enable the pressure in the downstream pipeline of the sampling pipeline control valve to reach the target pressure of the pressure display controller.
In the pressure adjustment in steps S2 and S3, nitrogen gas is supplied into the system while vacuumizing, so that the variability of the pressure in the system is small, the control of the pressure in the buffer tank and the system line is facilitated, and the pressure can reach the set pressure as soon as possible and be in a stable pressure state. Secondly, the pressure in the pipeline is regulated in stages, the opening state of each valve is controlled, the buffer tank is communicated with the vacuum pump and the first nitrogen inlet, and the pressure in the buffer tank is firstly regulated to reach a set pressure value; then, the opening state of each valve is controlled, so that the pipeline from the sampling pipeline control valve to the flow control valve is also communicated with the vacuum pump and the first nitrogen inlet, and the pressure is adjusted to the pressure set value. The pressure adjustment is carried out step by step, so that the phenomenon that the pressure range is adjusted once and is too large, the set pressure is inconsistent at all places is avoided, and the phenomenon that the speed is too high and the stable state is not easily reached when materials in the reaction system are extracted in vacuum is avoided.
The line evacuation stage comprises the steps of:
s4: when the pressure in the downstream pipeline of the sampling pipeline control valve reaches the target pressure of the pressure display controller, setting the target flow of the flow display controller to be 0.05-0.1% of the total flow of the main pipeline at the inlet of the reactor, opening the sampling pipeline control valve, enabling the gas-phase reaction materials in the sampling pipeline to sequentially flow through the sampling pipeline control valve, the flow control valve, the first automatic three-way valve, the second automatic three-way valve, the buffer tank and the vacuum pump under the action of pressure difference until the pipeline is emptied, and replacing the gas in the pipeline by the gas-phase reaction materials; in the replacement process, the flow display controller adjusts the opening of the flow control valve according to the set target flow to ensure that the flow in the pipeline is maintained at the set target flow; a small sampling amount is ensured through the flow controller, so that the influence on the reaction in the reactor is avoided; before the gas-phase reaction materials in the pipeline flow to the buffer tank, the gas-phase reaction materials are always in a heat preservation or electric tracing state so as to avoid the liquid condensation phenomenon; the buffer tank is in an ice bath state, so that heavier components such as benzene, ethylbenzene, styrene and the like are condensed into liquid, and non-condensable gas is discharged through a vacuumizing control valve and a vacuum pump.
The sampling analysis phase comprises the following steps:
s5: during sampling, the opening directions of the first automatic three-way valve and the second automatic three-way valve are adjusted, the gas chromatograph is connected into the system, the gas in the pipeline is replaced by the gas in the gas chromatograph after passing through the gas chromatograph, the gas chromatograph is filled with the gas after a period of time, and at the moment, the gas chromatograph performs component analysis on the gas.
In the steps, the first nitrogen inlet is always kept filled with nitrogen, the pressure display controller monitors the pressure in the buffer, the opening degree of the first nitrogen inlet valve is controlled, and whether nitrogen needs to be supplemented or not is determined so as to maintain the balance of the pressure in the buffer tank. The vacuum pump is used for providing power for the gas in the pipeline and maintaining the system in a negative pressure state, so that the vacuum pump is always in an open state in the steps until the gas chromatograph is filled with the sample gas and the sample gas is analyzed, and at the moment, the power does not need to be provided for the gas, so that the vacuum pump can be switched off or switched off after the analysis is finished.
The nitrogen purge stage comprises the following steps:
s6: after the analysis is completed, the sampling pipeline control valve, the first nitrogen inlet valve, the vacuumizing control valve and the vacuum pump are closed, the second nitrogen inlet valve is opened, sufficient nitrogen is supplemented into the system through the second nitrogen inlet until the pressure in the system reaches positive pressure, for example: and (4) enabling the pressure in the system to reach 150kPa, then, closing the second nitrogen inlet valve, opening the vacuumizing control valve and the vacuum pump, and pumping out the gas in the pipeline to empty the residual gas in the pipeline. In order to avoid the influence of residual gas in the system on subsequent measurement, sufficient nitrogen can be supplemented into the system through the second nitrogen inlet and then exhausted; repeating for multiple times until all residual gas is replaced.
When there are many sampling lines, in order to carry out the analysis to every sampling point, only switch on a sampling line at every turn, the gas in other sampling lines is in the stagnant state, if do not flow for a long time, can lead to gaseous phenomenon that condenses to appear, therefore, in order to avoid gas polymerization in the pipeline, the gas that will make many sampling lines often flows or replaces, at this moment, can open one or more sampling line control valves simultaneously, make the gaseous circulation in the pipeline, gas at this moment is not used for the sampling, need not to pass through gas chromatograph, consequently, parallelly connected the branch pipeline on gas chromatograph through first automatic three way valve and second automatic three way valve, be convenient for gaseous emission.
In addition, it is clear that the pressure in the pipeline is in a negative pressure state in the whole sampling analysis process.
The invention has the beneficial effects that:
1) in the prior art, a gas phase sample is condensed into a liquid phase for sampling. However, the prior art cannot collect and analyze the non-condensable components due to the presence of the non-condensable components (i.e., components that remain in the vapor phase after the condensation process). The method of the invention keeps the sample in a gas phase state all the time, and solves the defects of the prior art.
2) The prior art requires a long time for collecting a liquid phase sample and has a large collection quality, which interferes with the operation of a reaction system. The invention adopts a gas phase sampling mode, the displacement time of the sampling pipeline is short, the sampling quality is low, and the interference of the sampling process to the reaction system can be reduced.
3) The prior art mainly adopts manual operation, and intelligent degree is not high, has the operation complicacy, and the operator makes mistakes easily etc. not enough. In the method, the entire sampling and analysis system is integrated into the same control system. Set up automatic valve and instrument in necessary position, realized automatic sampling and advance a kind, solved the not enough of prior art.
Drawings
The invention is further illustrated by the following figures and examples.
FIG. 1 is a schematic structural diagram of the preferred embodiment of the present invention.
FIG. 2 is a schematic diagram of a prior art ethylbenzene dehydrogenation reaction system.
In the figure: 1. a first reactor, 2, a second reactor, 3, a heating furnace, 4, a heating furnace, 5, a temperature sensor, 6, a pressure transmitter, 7, a temperature sensor, 8, a pressure transmitter, 9, a temperature sensor, 10, a pressure transmitter, 11, a D point sampling pipeline control valve, 12, a B point sampling pipeline control valve, 13, a C point sampling pipeline control valve, 14, an A point sampling pipeline control valve, 15, a second nitrogen inlet valve, 16, a flow control valve, 17, a flow display controller, 18, a temperature sensor, 19, a pressure transmitter, 20, a first automatic three-way valve, 21, a second automatic three-way valve, 22, a gas chromatograph, 23, an oil bath device, 24, a vacuum pump, 25, a pressure display controller, 26, a liquid discharge control valve, 27, a buffer tank, 28, a branch air inlet valve, 29, a manual two-way valve, 30. the device comprises a first nitrogen inlet valve, a manual two-way valve, a second nitrogen inlet valve, a vacuum pumping control valve, a sampling pipeline at 33 and A points, a sampling pipeline at 34 and C points, a sampling pipeline at 35 and B points, a sampling pipeline at 36 and D points, a temperature sensor 37, a temperature sensor 38, a temperature display controller 39, a temperature sensor 40, a pressure transmitter 41, a first nitrogen inlet 42, a second nitrogen inlet 43 and a main pipeline.
Detailed Description
The present invention will now be described in detail with reference to the accompanying drawings. This figure is a simplified schematic diagram, and merely illustrates the basic structure of the present invention in a schematic manner, and therefore it shows only the constitution related to the present invention.
In this embodiment, taking an ethylbenzene dehydrogenation reaction system as an example, but not limited to the ethylbenzene dehydrogenation reaction system, as shown in fig. 1, the ethylbenzene dehydrogenation reaction system includes a first reactor 1 and a second reactor 2 connected in sequence, a material inlet of the first reactor 1 is directly connected to an upstream device, and a material after the reaction of the first reactor 1 enters the second reactor 2 for reaction, so that inlets and outlets of the two reactors have A, B, C and D four sampling points, wherein a and B are sampling points at inlets of the first reactor 1 and the second reactor 2, respectively, C and D are sampling points at outlets of the first reactor 1 and the second reactor 2, respectively, and four temperature sensors 5, 7, 9, and 18 and four pressure transmitters 6, 8, 10, and 19 are arranged on pipelines at the four sampling points to monitor temperature and pressure, respectively, and upstream pipelines at sampling points a and B of inlets of the first reactor 1 and the second reactor 2 are also arranged on pipelines at the sampling points a and B, respectively There are two furnaces 3 and 4, the reaction mass flowing out of the second reactor 2 being fed by means of a line to a downstream device.
In order to monitor and analyze the material components of the inlet and outlet pipelines of the two reactors, the serial negative pressure sampling analysis system of the invention comprises a sampling pipeline, an oil bath device, a gas phase analysis component, a buffer tank 27, a vacuum pump 24, a flow control component, a pressure control component and a nitrogen purging component, as shown in fig. 1, wherein the gas phase analysis component, the buffer tank 27 and the vacuum pump 24 are sequentially connected in series through pipelines to form a serial sampling analysis structure.
The number of the sampling pipelines corresponds to the number of the sampling points, and can be set according to the actual situation, in this embodiment, because the number of the sampling points is four, the corresponding sampling pipelines are also four, namely, the point A sampling pipeline 33, the point B sampling pipeline 35, the point C sampling pipeline 34 and the point D sampling pipeline 36, one end of each sampling pipeline is respectively connected to A, B, C and four sampling points D of the reactor for sampling and inputting of gas phase reaction materials, the other end of each sampling pipeline is respectively connected to four sampling pipeline control valves after passing through the oil bath device 23, namely, the point A sampling pipeline control valve 14, the point B sampling pipeline control valve 12, the point C sampling pipeline control valve 13 and the point D sampling pipeline control valve 11, the other ends of the four sampling pipeline control valves are converged together to form the main pipeline 43, during sampling and analyzing, the sampling and analyzing can be performed on the sampling points as long as the corresponding sampling pipeline control valves are opened, and the different sampling pipeline control valves are switched to realize the analysis of the gas components of a plurality of sampling points, and as the optimal selection of four sampling pipeline control valves, automatic two-way valves are adopted.
The oil bath device 23 is arranged on the path of the sampling pipeline, the temperature of the materials in the sampling pipeline is reduced to a certain proper range from the original temperature of above 580 ℃ after the temperature is controlled by the oil bath, the reaction materials are not condensed at the temperature, the polymerization phenomenon of the styrene is not obvious, and the preferable temperature is 120-150 ℃. Preferably, the oil bath device 23 is a constant temperature oil bath which has a temperature display and temperature control function, such as monitoring and adjusting the temperature of the oil bath by using a temperature sensor 37 and a temperature display controller 38. The collected main pipeline 43 is provided with a temperature sensor 39 and a pressure transmitter 40, which are respectively used for monitoring the temperature and the pressure of the gas therein.
In order to control the flow in the sampling pipeline within a relatively small flow range, the main pipeline 43 is further provided with a flow control assembly, the flow control assembly comprises a flow control valve 16 and a flow display controller 17, wherein the flow control valve 16 preferably adopts an automatic two-way valve, the flow control valve 16 is arranged on the main pipeline 43 at the upstream of the gas phase analysis assembly, the flow display controller 17 is in signal connection with a control end of the flow control valve 16, the flow display controller 17 is used for setting and displaying the flow and monitoring the flow in the sampling main pipeline 43, and the opening degree of the flow control valve 16 is adjusted according to the set flow and the monitored flow in the main pipeline 43. When the device is used, the set value of the flow display controller 17 is automatically set to be a lower value so as to avoid the phenomenon that the material in the reaction system is pumped in vacuum at an excessive speed later.
And a nitrogen purging assembly is further arranged on the main pipeline 43 at the upstream of the flow control assembly, the nitrogen purging assembly comprises a second nitrogen inlet 42 and a second nitrogen inlet valve 15, and the second nitrogen inlet 42 is connected to the main pipeline 43 at the upstream of the flow control assembly through the second nitrogen inlet valve 15. The second nitrogen inlet valve 15 is preferably an automatic two-way valve. And the sampling gas at the previous sampling point in the system is exhausted through the nitrogen purging assembly, so that continuous multipoint sampling analysis is facilitated.
The main pipeline 43 is connected to a gas analysis assembly, the gas analysis assembly comprises a gas chromatograph 22, a first automatic three-way valve 20 and a second automatic three-way valve 21, the gas chromatograph 22 is connected in series on the sampling main pipeline 43 through the first automatic three-way valve 20 and the second automatic three-way valve 21, and two ends of the gas chromatograph 22 are further connected with a branch pipeline in parallel through the first automatic three-way valve 21 and the second automatic three-way valve 22. One end of the first automatic three-way valve 20 connected with the sampling main pipeline 43 is used as a gas inlet and outlet end of the gas analysis component, and one end of the second automatic three-way valve 21 connected with the buffer tank 27 is used as the other gas inlet and outlet end of the gas analysis component, when the gas chromatograph 22 is not needed, the opening directions of the first automatic three-way valve 20 and the second automatic three-way valve 21 are downward, and the gas chromatograph 22 is bypassed, so that the gas chromatograph 22 is not connected into the system, and a branch pipeline is connected into the system, at the moment, gas in the sampling pipeline can be updated and replaced, and the gas aggregation phenomenon is avoided; when analysis is needed, the first automatic three-way valve 20 and the second automatic three-way valve 21 are opened upwards, so that the gas chromatograph 22 is connected into the system. (the "up" and "down" are used herein with respect to the orientation and position of the three-way valve shown in FIG. 1, not an absolute position.)
The other gas phase inlet and outlet end of the gas phase analysis assembly is connected to the buffer tank 27 through a pipeline, an outlet of the buffer tank 27 is connected to the vacuum pump 24 through a pipeline, in order to facilitate on-off control of gas flow in the pipeline, a vacuumizing control valve 32 is arranged on the pipeline between the buffer tank 27 and the vacuum pump 24, a liquid discharge pipe is arranged at the bottom of the buffer tank 27, and a liquid discharge control valve 26 is arranged on the liquid discharge pipe. Since the sampling is automatically controlled and the discharge of the condensate in the buffer tank 27 is not necessarily automatically controlled, it is preferable to use an automatic two-way valve for the vacuum control valve 32 and a manual two-way valve for the liquid discharge control valve 26.
The buffer tank 27 is also connected with a pressure control assembly for monitoring the pressure in the pipeline upstream and downstream of the gas phase analysis assembly and in the buffer tank 27 and controlling the air inflow of the first nitrogen inlet 41 according to the monitored pressure; in order to control the pressure adjustment with smaller pressure fluctuation, the pressure control assembly comprises a pressure display controller 25 and a first nitrogen inlet valve 30, preferably, the first nitrogen inlet valve 30 adopts an automatic two-way valve, the first nitrogen inlet valve 30 is connected in series on a pipeline between the buffer tank 27 and the first nitrogen inlet 41, the pressure display controller 25 is in signal connection with a control end of the first nitrogen inlet valve 30, the pressure display controller 25 is used for setting and displaying the pressure and monitoring the pressure in the buffer tank 27, and the opening degree of the first nitrogen inlet valve 30 is adjusted according to the set pressure and the monitored pressure in the buffer tank 27. The pressure control component enables the pressure in the sampling analysis system and the pressure in the reactor and the main pipeline thereof to generate a smaller pressure difference, so that the sampling gas can be ensured to enter the sampling analysis system under the action of the pressure difference, and the buffer tank 27 can also prevent suck-back and protect the vacuum pump 24. In order to improve the stability of the nitrogen-containing gas, a manual two-way valve 29 and a manual two-way valve 31 are respectively arranged on the pipelines at the upstream and downstream of the first nitrogen inlet valve 30, wherein the manual two-way valve is used for directly cutting off the gas flow of the first nitrogen inlet 41, and the first nitrogen inlet valve 30 is used for regulating and controlling the flow of nitrogen; a branch pipeline is further connected in parallel on the main pipeline formed by the first nitrogen inlet valve 30 and the manual two- way valves 29 and 31, and a manual two-way valve is arranged on the branch pipeline and serves as a branch air inlet valve 28. When the first nitrogen inlet valve 30 and the manual two- way valves 29 and 31 on the main pipeline are in failure and the nitrogen cannot be introduced, the branch gas inlet valve 28 on the branch pipeline is opened to introduce the nitrogen.
The pipelines in front of the buffer tank 27 are all provided with a heat preservation or heating device. The sampling gas is always in a heat preservation or electric heat tracing state, and the sampling material is always kept in a gas state. In order to avoid the discharged gas from polluting the environment, the device also comprises an ice bath device, wherein the buffer tank is arranged in the ice bath device, and the temperature range of the ice bath is 5-15 ℃. The buffer tank is in ice bath, so that heavier components such as benzene, ethylbenzene, styrene and the like are condensed into liquid without being discharged.
A series connection type vacuum sampling analysis method comprises the vacuum sampling analysis system, and the method is mainly divided into five stages, namely a parameter setting stage, a pressure adjusting stage, a pipeline emptying stage, a sampling analysis stage and a nitrogen purging stage, wherein an A sampling point is taken as an example to explain the sampling method.
The time to start the sampling and analysis operations was manually set to 12 o' clock at 10 am. Samples were taken at the inlet of the first reactor at 12 o' clock for analysis. All the following operations are automatically performed by the control system automatic control hardware device.
At 11 am, the automatic control system ensured that the valves were in the following states:
the valve is in a closed state: 11,12,13,14,15,16,32,26, 28;
the valve is in an open state: 29, 31;
the opening directions of the first automatic three-way valve 20 and the second automatic three-way valve 21 are: downward, i.e., bypassing the gas chromatograph 22.
At 11:30 AM, pressure transmitter 6 has a value of 60 kPa. The vacuum pump 24 is automatically turned on, the vacuum-pumping control valve 32 is automatically turned on, and the target value of the pressure display controller 25 is automatically set to be 55kPa, which is the value obtained by subtracting 5kPa from the value of the pressure transmitter 6. The first nitrogen inlet valve 30 will automatically adjust the opening to change the amount of nitrogen make-up through the first nitrogen inlet valve 30 to bring the pressure in the buffer tank 27 to the set value of the pressure display controller 25, i.e., 55 kPa.
After the last operation (after 10 minutes expected), the set value of the flow indicator controller 17 is automatically set to a lower value, i.e. 20mL/min, so that the flow control valve 16 is adjusted to open its opening until the feedback value of the pressure transmitter 40 is equal to the value of the pressure indicator controller 25.
After the last step of operation is completed, the set value of the flow display controller 17 is automatically set to a lower value, i.e. 20mL/min, so as to avoid the excessive speed of the vacuum pumping of the materials in the reaction system.
The A-point sampling line is then automatically opened to control valve 14. The gas in the sampling line 33 at point a will flow under the pressure difference to the valve 14, then through the valve 16, the valve 20, the valve 21, the buffer tank 27, the valve 32, and the vacuum pump 24 in sequence until it is exhausted. The gas is kept warm or electrically heated until it flows into the buffer tank 27, so as to avoid the condensation of the liquid. The temperature of electric tracing of the pipeline is 150 ℃. The buffer tank 27 is placed in an ice bath at a temperature of 5 ℃, so that heavier components such as benzene, ethylbenzene, styrene and the like are condensed into liquid, and non-condensable gas is discharged through a valve 32 and a vacuum pump 24.
After a certain time t1, i.e. 10 minutes of displacement, the lines were filled with sample gas. The states of the first automatic three-way valve 20 and the second automatic three-way valve 21 are automatically adjusted to the upward positions, and the gas is passed through the gas chromatograph 22 to replace the lines in the gas chromatograph 22. After a certain time t2, i.e. 5 minutes, program control automatically starts the gas chromatograph 22 to feed for component analysis.
After the sample introduction is completed, the program controls the automatic closing valve 14, the automatic closing valve 30 and the automatic closing valve 32. The time at this point is about 12 pm.
The sampling and online analysis of the other three sampling ports is similar.
The sampling method can be suitable for sampling the ethylbenzene dehydrogenation reaction discussed above and can also be deduced to be used for sampling other negative pressure reaction systems.
The sampling analysis system of the invention:
(1) the sample is kept in a gas phase state before entering the gas chromatograph 22, so that gas-liquid two phases are avoided, and the sample is pumped into the gas chromatograph 22 through the vacuum pump 24, so that vacuum and online sampling and analysis are realized.
The temperature of the gas phase sample is cooled from above 580 ℃ to 120-150 ℃, and the temperature is reduced to a temperature which can be endured by the gas chromatograph 22 and a conventional valve.
And a full-automatic design is adopted. The operator only needs to set the sampling time, and other operations can be automatically controlled and executed by the computer control system.
A flow display controller 17 is provided to avoid excessive speed during vacuum pumping and interference with the reaction system.
A nitrogen purge line is provided so that the reaction gas remaining in the line is purged.
A pressure sensor (pressure transmitter) and a pressure display controller 25 are provided so that the pressure value of the pipeline can be automatically adjusted.
The sampling pipelines are all thin in pipe diameter so as to reduce dead volume in the sampling pipelines as much as possible. For example, the inner diameter of the sampling line is no more than 5% of the inner diameter of the main line.
The valves 11,12,13,14 are arranged on the pipelines after cooling instead of the valves arranged in the high-temperature pipelines 33,34,35,36, so that only the conventional valves are needed, and the hardware investment and the maintenance difficulty are reduced.
A nitrogen make-up bypass, i.e. nitrogen entering through valve 29, is provided in buffer tank 27 upstream of vacuum pump 24 to prevent air from entering the sampling system.
In light of the foregoing description of preferred embodiments in accordance with the invention, it is to be understood that numerous changes and modifications may be made by those skilled in the art without departing from the scope of the invention. The technical scope of the present invention is not limited to the contents of the specification, and must be determined according to the scope of the claims.
Claims (10)
1. A serial-type negative pressure sampling analytic system which characterized in that: the device comprises a sampling pipeline, an oil bath device, a gas phase analysis assembly, a buffer tank, a vacuum pump, a flow control assembly and a pressure control assembly, wherein one end of the sampling pipeline is connected to a sampling point of a reactor and used for sampling and inputting gas phase reaction materials, the other end of the sampling pipeline is connected to one end of a sampling pipeline control valve after passing through the oil bath device, the other end of the sampling pipeline control valve is connected to a gas phase inlet and outlet end of the gas phase analysis assembly through a pipeline, the flow control assembly is arranged on the pipeline between the sampling pipeline control valve and the gas phase analysis assembly, the other gas phase inlet and outlet end of the gas phase analysis assembly is connected to the buffer tank through a pipeline, an outlet of the buffer tank is connected to the vacuum pump through a pipeline, an inlet of the buffer tank is connected to a first nitrogen inlet through a pipeline, and the pressure control assembly is, controlling the air inflow of the first nitrogen inlet according to the monitored pressure; the gas phase analysis assembly, the buffer tank and the vacuum pump are sequentially connected in series through pipelines to form a serial-type sampling analysis structure.
2. The in-line negative pressure sampling analysis system of claim 1, wherein: the gas analysis subassembly includes gas chromatograph, first automatic three way valve and the automatic three way valve of second, gas chromatograph establishes ties on the pipeline between buffer tank and flow control subassembly through first automatic three way valve and the automatic three way valve of second, and gas chromatograph's both ends are still parallelly connected a branch road pipeline through first automatic three way valve and the automatic three way valve of second.
3. The in-line negative pressure sampling analysis system of claim 1, wherein: the flow control assembly comprises a flow control valve and a flow display controller, the flow control valve is arranged on a pipeline on the upstream of the gas phase analysis assembly, the flow display controller is in signal connection with a control end of the flow control valve, the flow display controller is used for setting and displaying flow, monitoring the flow in the sampling pipeline, and adjusting the opening degree of the flow control valve according to the set flow and the monitored flow in the pipeline.
4. The in-line negative pressure sampling analysis system of claim 1, wherein: the pressure control assembly comprises a pressure display controller and a first nitrogen inlet valve, the first nitrogen inlet valve is connected in series on a pipeline between the buffer tank and the first nitrogen inlet, the pressure display controller is connected with a control end signal of the first nitrogen inlet valve, the pressure display controller is used for setting and displaying pressure and monitoring the pressure in the buffer tank, and the opening degree of the first nitrogen inlet valve is adjusted according to the set pressure and the monitored pressure in the buffer tank.
5. The in-line negative pressure sampling analysis system of claim 4, wherein: and the pipeline on the upper and lower reaches of the first nitrogen inlet valve is respectively provided with a manual two-way valve, a branch pipeline is further connected in parallel on the main pipeline formed by the first nitrogen inlet valve and the manual two-way valve, and a branch air inlet valve is arranged on the branch pipeline.
6. The in-line negative pressure sampling analysis system of claim 1, wherein: the pipeline between buffer tank and the vacuum pump is equipped with a vacuum pumping control valve, and the buffer tank bottom is equipped with the fluid-discharge tube, just be equipped with a drainage control valve on the fluid-discharge tube.
7. The in-line negative pressure sampling analysis system of any one of claims 1-6, wherein: the nitrogen purging assembly comprises a second nitrogen inlet and a second nitrogen inlet valve, and the second nitrogen inlet is connected to a main pipeline at the upstream of the flow control assembly through a pipeline through the second nitrogen inlet valve.
8. The in-line negative pressure sampling analysis system of claim 7, wherein: the ice bath device is also included, the buffer tank is arranged in the ice bath device, and the temperature range of ice bath is 5-15 ℃.
9. A tandem type vacuum sampling analysis method is characterized in that: a vacuum sampling analysis system comprising any of claims 1-8, further comprising the steps of:
s1: adjusting the on-off state of a valve in the system to enable the sampling pipeline control valve, the second nitrogen inlet valve, the flow control valve, the vacuumizing control valve and the liquid discharge control valve to be in a closed state; a valve on a branch pipeline between the first nitrogen inlet and the buffer tank is in a closed state; adjusting the directions of a first automatic three-way valve and a second automatic three-way valve in the gas analysis assembly to enable the gas chromatograph to be in a state of not being connected with a pipeline between the flow control valve and the buffer tank;
s2: opening a vacuum pump and a vacuumizing control valve to vacuumize, setting a target pressure value of a pressure display controller to be smaller than a pressure value at an inlet of an upstream reactor, introducing nitrogen into the buffer tank through a main line of a first nitrogen inlet, monitoring the pressure in the buffer tank by the pressure display controller, and adjusting the opening of the first nitrogen inlet valve according to the monitored pressure and the target pressure value to enable the pressure in the buffer tank to reach and maintain the target pressure value;
s3: when the pressure in the buffer tank reaches a target pressure value, opening the flow control valve to enable the pressure in a downstream pipeline of the sampling pipeline control valve to reach the target pressure of the pressure display controller;
s4: when the pressure in the downstream pipeline of the sampling pipeline control valve reaches the target pressure of the pressure display controller, setting the target flow of the flow display controller to be 0.05-0.1% of the total flow of the main pipeline at the inlet of the reactor, opening the sampling pipeline control valve, enabling the gas-phase reaction materials in the sampling pipeline to sequentially flow through the sampling pipeline control valve, the flow control valve, the first automatic three-way valve, the second automatic three-way valve, the buffer tank and the vacuum pump under the action of pressure difference until the pipeline is emptied, and replacing the gas in the pipeline by the gas-phase reaction materials; in the replacement process, the flow display controller adjusts the opening of the flow control valve according to the set target flow to ensure that the flow in the pipeline is maintained at the set target flow;
s5: during sampling, adjusting the opening directions of the first automatic three-way valve and the second automatic three-way valve, enabling the gas chromatograph to be connected into the system, enabling the sample gas in the pipeline to pass through the gas chromatograph to replace the gas in the gas chromatograph, and filling the gas chromatograph with the sample gas after a period of time, wherein at the moment, the gas chromatograph performs component analysis on the sample gas;
s6: and after the analysis is finished, closing the sampling pipeline control valve, the first nitrogen inlet valve, the vacuumizing control valve and the vacuum pump, opening the second nitrogen inlet valve, supplementing nitrogen into the system through the second nitrogen inlet until the pressure in the system reaches positive pressure, then closing the second nitrogen inlet valve, opening the vacuumizing control valve and the vacuum pump, and pumping out the gas in the pipeline to empty the residual sample gas in the pipeline.
10. The inline vacuum sampling analysis method of claim 9, wherein: step S0 is further included before step S1: the control system sets the operation time of automatic sampling and analysis, and controls the sampling analysis system to automatically execute sampling according to the set time.
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