CN111855259A - Online sample collection system and method - Google Patents
Online sample collection system and method Download PDFInfo
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- CN111855259A CN111855259A CN202010837155.6A CN202010837155A CN111855259A CN 111855259 A CN111855259 A CN 111855259A CN 202010837155 A CN202010837155 A CN 202010837155A CN 111855259 A CN111855259 A CN 111855259A
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- 238000000034 method Methods 0.000 title claims abstract description 22
- 238000005070 sampling Methods 0.000 claims abstract description 125
- 238000006243 chemical reaction Methods 0.000 claims abstract description 109
- 239000007789 gas Substances 0.000 claims abstract description 76
- 238000010926 purge Methods 0.000 claims abstract description 68
- 239000011343 solid material Substances 0.000 claims abstract description 41
- 239000011261 inert gas Substances 0.000 claims abstract description 27
- 238000001514 detection method Methods 0.000 claims abstract description 25
- 238000007664 blowing Methods 0.000 claims abstract description 17
- 238000005086 pumping Methods 0.000 claims abstract description 15
- 239000002245 particle Substances 0.000 claims description 19
- 239000007787 solid Substances 0.000 claims description 13
- 230000009471 action Effects 0.000 claims description 11
- 230000001105 regulatory effect Effects 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 238000004891 communication Methods 0.000 claims description 4
- 239000012495 reaction gas Substances 0.000 claims description 3
- 238000012512 characterization method Methods 0.000 abstract description 5
- 238000010408 sweeping Methods 0.000 description 6
- 230000007246 mechanism Effects 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 4
- 239000010410 layer Substances 0.000 description 4
- 230000008569 process Effects 0.000 description 3
- 238000005299 abrasion Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005485 electric heating Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000007769 metal material Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
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- 238000009413 insulation Methods 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 230000035772 mutation Effects 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000000126 substance 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B9/00—Cleaning hollow articles by methods or apparatus specially adapted thereto
- B08B9/02—Cleaning pipes or tubes or systems of pipes or tubes
- B08B9/027—Cleaning the internal surfaces; Removal of blockages
- B08B9/032—Cleaning the internal surfaces; Removal of blockages by the mechanical action of a moving fluid, e.g. by flushing
- B08B9/0321—Cleaning the internal surfaces; Removal of blockages by the mechanical action of a moving fluid, e.g. by flushing using pressurised, pulsating or purging fluid
- B08B9/0328—Cleaning the internal surfaces; Removal of blockages by the mechanical action of a moving fluid, e.g. by flushing using pressurised, pulsating or purging fluid by purging the pipe with a gas or a mixture of gas and liquid
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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
- G01N33/0009—General constructional details of gas analysers, e.g. portable test equipment
- G01N33/0011—Sample conditioning
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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
- 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
-
- 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
- G01N33/0021—Sample conditioning involving the use of a carrier gas for transport to the sensor
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Abstract
The invention discloses an online sample collection system and a method, belonging to the technical field of sample detection, wherein the online sample collection system comprises a first blowing system capable of conveying inert gas, a sampling structure, a second blowing system, a first switching structure, a second switching structure and a vacuum pumping system which are sequentially connected through a pipeline, the first blowing system is connected with the pipeline between the first switching structure and the second switching structure, the sampling structure is connected with the second switching structure, and the sampling structure is provided with an exhaust port capable of being opened and closed; the first switching structure is connected with a sample introduction pipeline, the sample introduction pipeline can extend into the solid material of the reaction device, and the second purging system can convey gas of the same type as at least one gas in the reaction device. Compact structure can realize continuous sampling, avoids remaining solid material in pipeline and switching structure, and collection efficiency is high. And the freshness of the collected sample and the accuracy of the subsequent sample characterization result can be ensured.
Description
Technical Field
The invention relates to the technical field of sample detection, in particular to an online sample collection system and method.
Background
In the process industry, the characterization of the material reaction process is the basis for researching the reaction mechanism, optimizing the reaction parameters, improving the product yield and controlling the reaction process. At present, for the research on the reaction process characterization of process industrial substances, devices such as a thermogravimetric analyzer, a fixed bed/fluidized bed reactor, an electric heating grid reactor, a curie point reactor and the like are mostly used, and the on-line or off-line detection of gas-phase products in the reaction process is realized. Although the method can analyze kinetic parameters in the reaction process and control the reaction process to a certain extent, the method cannot acquire solid particle substances in the reaction process, and cannot characterize solid particles, so that the method cannot realize the capture of 'mutation points' in the reaction process and the exploration of mechanism change in the conversion process.
Aiming at the problems, a particle collection system aiming at solid particles appears, but the existing particle collection system has a complex structure, the solid particles are often remained in pipelines and switching structures after sampling, the continuous sampling operation is not suitable, and the collection efficiency is low; and the remaining solid particles can wear the switching structure, reducing its service life.
Disclosure of Invention
The invention aims to provide an online sample collection system and method, and aims to solve the problems that in the prior art, a particle collection system is complex in structure, solid particles are often left in pipelines and components after sampling, the continuous sampling operation is not suitable, the collection efficiency is low, and a switching structure is easy to wear.
As the conception, the technical scheme adopted by the invention is as follows:
an online sample collection system comprises a first blowing system, a sampling structure, a second blowing system, a first switching structure, a second switching structure and a vacuum pumping system, wherein the first blowing system and the sampling structure can convey inert gas, and the second blowing system, the first switching structure, the second switching structure and the vacuum pumping system are sequentially connected through a pipeline; the first switching structure is connected with a sample introduction pipeline, the sample introduction pipeline can extend into the solid material of the reaction device, and the second purging system can convey gas of the same type as at least one gas in the reaction device;
the first switching structure can selectively enable the reaction device to be communicated with the second purging system or the second switching structure, the second switching structure can selectively enable the sampling structure to be communicated with the first switching structure or the vacuumizing system, and the vacuumizing system is configured to vacuumize the sampling structure to enable solid materials in the reaction device to enter the sampling structure under the action of pressure difference.
Further, the first purging system comprises a first gas storage tank, a first flow regulating structure and a first buffer tank which are connected in sequence, inert gas is filled in the first gas storage tank, and the first buffer tank is connected to a pipeline between the first switching structure and the second switching structure.
Further, the second purging system comprises a second gas storage tank, a second flow rate adjusting structure and a second buffer tank which are sequentially connected, wherein the second gas storage tank is filled with gas of the same type as at least one gas in the reaction device, and the second buffer tank is connected to the first switching structure.
Further, the vacuum pumping system comprises a vacuum pump, a first filter and a vacuum degree regulating valve which are sequentially connected, and the vacuum degree regulating valve is connected to the second switching structure through a pipeline.
Furthermore, the online sample collection system further comprises a communicating structure, wherein the communicating structure is provided with a first interface, a second interface and a third interface which are communicated with each other in pairs, the first interface is communicated with the first blowing system, the second interface is communicated with the first switching structure, and the third interface is communicated with the second switching structure.
Further, online sample collection system still includes gaseous detecting system, gaseous detecting system is including the gaseous detection device, dewatering structure and the second filter that connect gradually, the second filter can communicate in through the pipeline reaction unit.
Further, the gas detection system further comprises a three-way valve, the three-way valve is provided with a first port, a second port and a third port, the first port is communicated with the water removal structure, the second port is communicated with the gas detection device, and the third port is an evacuation port.
Furthermore, the part of the sample feeding pipeline extending out of the reaction device, the pipeline between the first switching structure and the second switching structure and the pipeline between the second switching structure and the sampling structure are all wrapped with heat insulation layers.
In order to achieve the above object, the present invention further provides an online sample collection method, which is applied to the online sample collection system in any of the above schemes,
further, the online sample collection method comprises:
switching the second switching structure to a sampling structure to be communicated with a vacuumizing system, vacuumizing the sampling structure, adjusting the vacuum degree of the sampling structure through a vacuum degree adjusting valve until the pressure in the sampling structure is within a preset pressure range, and stopping vacuumizing;
the reaction device is communicated with the sampling structure through a connecting pipeline by adjusting the first switching structure and the second switching structure, and solid materials in the reaction device enter the sampling structure along the pipeline under the action of pressure difference between the reaction device and the sampling structure;
adjusting the second switching structure to communicate the sampling structure with the vacuum pumping system, and vacuumizing the sampling structure again to pump out the reaction gas entering the sampling structure from the reaction device, and simultaneously conveying inert gas into a connecting pipeline between the reaction device and the sampling structure through the first purging system to blow back residual solid particles in a part of the connecting pipeline between the connecting point of the first purging system and the connecting pipeline and the reaction device into the reaction device;
stopping vacuumizing the sampling structure, switching the first switching structure to a second purging system to be communicated with the reaction device, and purging the sample introduction pipeline through the second purging system; simultaneously, switching the second switching structure to a first blowing system to be communicated with the sampling structure, opening an exhaust port of the sampling structure, and conveying inert gas into a connecting pipeline between the reaction device and the sampling structure through the first blowing system so as to blow residual solid particles in a part of the connecting pipeline between the connecting point of the first blowing system and the connecting pipeline and the sampling structure into the sampling structure by using inert atmosphere;
and closing the first purging system, replacing the sampling structure and keeping the second purging system in an opening state.
Further, the online sample collection method further comprises: the gas in the reaction device enters the gas detection device after being filtered and dewatered.
The invention has the beneficial effects that:
the invention provides an online sample collection system and a method, wherein the online sample collection system can vacuumize a sampling structure through a vacuumizing system, so that a small amount of solid materials in a reaction device can enter the sampling structure under the action of pressure difference on one hand, and gas entering the sampling structure from the reaction device can be pumped out on the other hand, and the solid materials are prevented from continuously reacting; through setting up second system and the first system of sweeping sweeps, can switch the structure to pipeline, first switching structure and the second of this online sample system and sweep completely, avoid remaining solid material in the pipeline and in the switching structure, and can also carry inert gas in to the sampling structure through first system of sweeping to protect the solid material in the sampling structure. This online sample collection system, compact structure can realize continuous sampling, and collection efficiency is high, and can avoid remaining solid material in pipeline and switching structure, guarantees the new freshness of gathering the sample and the accuracy of follow-up sample characterization result. In addition, the abrasion of residual particles in the switching structure to the switching structure when the switching structure is repeatedly used can be avoided, and the service life of the switching structure is prolonged.
Drawings
Fig. 1 is a schematic structural diagram of an on-line sample collection system provided by the present invention.
In the figure:
1. a first purge system; 11. a first gas storage tank; 12. a first flow regulating structure; 13. a first buffer tank; 2. a sampling structure; 21. an exhaust port; 3. a second purge system; 31. a second gas storage tank; 32. a second flow regulating structure; 33. a second buffer tank; 4. a first switching structure; 5. a second switching structure; 6. a vacuum pumping system; 61. a vacuum pump; 62. a first filter; 63. a vacuum degree regulating valve; 7. a reaction device; 8. a communicating structure; 9. a gas detection system; 91. a gas detection device; 92. a dewatering structure; 93. a second filter; 94. a three-way valve; 10. and a sample introduction pipeline.
Detailed Description
In order to make the technical problems solved, the technical solutions adopted and the technical effects achieved by the present invention clearer, the technical solutions of the present invention are further described below by way of specific embodiments with reference to the accompanying drawings. It is to be understood that the specific embodiments described herein are merely illustrative of the invention and are not limiting of the invention. It should be further noted that, for the convenience of description, only some but not all of the elements associated with the present invention are shown in the drawings.
In the description of the present invention, unless expressly stated or limited otherwise, the terms "connected," "connected," and "fixed" are to be construed broadly, e.g., as meaning permanently connected, removably connected, or integral to one another; can be mechanically or electrically connected; either directly or indirectly through intervening media, either internally or in any other relationship. The specific meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art.
In the present invention, unless otherwise expressly stated or limited, "above" or "below" a first feature means that the first and second features are in direct contact, or that the first and second features are not in direct contact but are in contact with each other via another feature therebetween. Also, the first feature being "on," "above" and "over" the second feature includes the first feature being directly on and obliquely above the second feature, or merely indicating that the first feature is at a higher level than the second feature. A first feature being "under," "below," and "beneath" a second feature includes the first feature being directly under and obliquely below the second feature, or simply meaning that the first feature is at a lesser elevation than the second feature.
In the description of the present embodiment, the terms "upper", "lower", "left", "right", and the like are used based on the orientations and positional relationships shown in the drawings only for convenience of description and simplification of operation, and do not indicate or imply that the referred device or element must have a specific orientation, be configured and operated in a specific orientation, and thus, should not be construed as limiting the present invention. Furthermore, the terms "first" and "second" are used only for descriptive purposes and are not intended to have a special meaning.
As shown in fig. 1, the present embodiment provides an online sample collection system, which includes a first purging system 1 capable of conveying an inert gas, a sampling structure 2, a second purging system 3, a first switching structure 4, a second switching structure 5, and a vacuum pumping system 6, which are sequentially connected through a pipeline, wherein the first purging system 1 is connected in a pipeline between the first switching structure 4 and the second switching structure 5, the sampling structure 2 is connected to the second switching structure 5, the sampling structure 2 has an exhaust port 21 capable of being opened and closed, the first switching structure 4 is connected to a sample introduction pipeline 10, the sample introduction pipeline 10 can extend into a solid material of a reaction device 7, and the second purging system 3 can convey a gas of the same type as at least one gas in the reaction device 7; the first switching structure 4 can selectively communicate the reaction device 7 with the second switching structure 5 or the second purging system 3, and the second switching structure 5 can selectively communicate the sampling structure 2 with the first switching structure 4 or the vacuum pumping system 6. The vacuum pumping system 6 can pump vacuum to the sampling structure 2, so that the solid material in the reaction device 7 enters the sampling structure 2 under the action of the pressure difference between the reaction device 7 and the sampling structure 2.
It should be noted that the solid material in the reaction device 7 is a catalyst or a component participating in the reaction, and the gas in the reaction device 7 is a component participating in the reaction or a gas product generated by the reaction. In the present embodiment, the first switching structure 4 and the second switching structure 5 are preferably three-way valves. Furthermore, in the present embodiment, the sampling structure 2 is a collection bottle having a vent 21.
It will be appreciated that when collecting solid material, the sampling structure 2 may first be connected to the evacuation system 6 via the second switching structure 5, the exhaust port 21 of the sampling structure 2 is closed, and then the sampling structure 2 is evacuated via the evacuation system 6. Then make second switching structure 5 communicate reaction unit 7 through first switching structure 4, make sampling structure 2 communicate first switching structure 4 through second switching structure 5, under the effect of the pressure differential between reaction unit 7 and sampling structure 2, the solid material in the reaction unit 7 enters into in the sampling structure 2 along the pipeline to the realization is to the collection of solid material. In addition, when sampling structure 2 and evacuation system 6 communicate, evacuation system 6 can be taken out the gas that enters into sampling structure 2 by reaction unit 7, prevents that solid material from continuing to react, guarantees the accuracy of follow-up sign result. In addition, not only can sweep the pipeline through first purge system 1, can also carry inert gas to in the sampling structure 2 to protect the solid material in the sampling structure 2, be convenient for the seal up of solid material. Through second purge system 3, can blow back into reaction unit 7 with remaining solid material in advancing kind pipeline 10 to and avoid when the sampling is intermittent, the material in reaction unit 7 gets into and advances kind pipeline 10 and take place the reaction, causes to advance kind pipeline 10 and blocks up.
Specifically, as shown in fig. 1, the first purging system 1 includes a first gas storage tank 11, a first flow rate adjusting structure 12, and a first buffer tank 13 connected in sequence, the first gas storage tank 11 is filled with an inert gas, and the first buffer tank 13 is connected in a pipeline between the first switching structure 4 and the second switching structure 5. The flow of the inert gas delivered to the outside from the first gas storage tank 11 can be adjusted through the first flow adjusting structure 12; the first buffer tank 13 can buffer the inert gas, reduce the purge pressure, and prevent particles from being ejected from the reaction device 7 or the sampling structure 2 due to too high purge pressure.
Further, the online sample collection system further comprises a communicating structure 8, wherein the communicating structure 8 is provided with a first interface, a second interface and a third interface which are communicated with each other pairwise, the first interface is communicated with the first buffer tank 13, the second interface is communicated with the first switching structure 4, and the third interface is communicated with the second switching structure 5. Of course, in other embodiments, the communication structure 8 may be a three-way valve, that is, the communication structure 8 can selectively communicate the first purging system 1 with the first switching structure 4 or the second switching structure 5. When the first purging system 1 is made to communicate with the first switching structure 4, and the first switching structure 4 communicates with the reaction device 7, the first purging system 1 can purge the solid materials remaining in the pipeline between the communicating structure 8 and the first switching structure 4 and the sample introduction pipeline 10 back into the reaction device 7. When making first system 1 of sweeping and switching over structure 5 of second intercommunication, and second switching over structure 5 intercommunication sampling structure 2, first system 1 of sweeping and can blow remaining solid material in the pipeline between communicating structure 8 and the sampling structure 2 to sampling structure 2 in, carry inert gas to protect the solid material in the sampling structure 2 simultaneously.
Referring again to fig. 1, the second purging system 3 includes a second gas storage tank 31, a second flow rate regulating structure 32 and a second buffer tank 33 connected in sequence, the second gas storage tank 31 is filled with a gas of the same type as at least one gas in the reaction device 7, and the second buffer tank 33 is connected to the first switching structure 4. The flow rate of the inert gas delivered to the outside from the second gas storage tank 31 can be adjusted by the second flow rate adjusting structure 32; the second buffer tank 33 can reduce the pressure of the gas supplied from the second gas storage tank 33 into the sampling device 7, thereby preventing particles from being ejected from the reaction device 7 due to an excessively high purge pressure.
The vacuum pumping system 6 includes a vacuum pump 61, a first filter 62 and a vacuum degree adjusting valve 63 connected in sequence, and the vacuum degree adjusting valve 63 is connected to the second switching structure 5 through a pipeline. When the second switching mechanism 5 makes the sampling mechanism 2 and the vacuum degree adjusting valve 63 communicate, the vacuum pump 61 can evacuate the sampling mechanism 2. Further, the output power of the vacuum pump 61 can be adjusted by the vacuum degree adjusting valve 63, so that the adjustment and control of the vacuum degree in the sampling structure 2 are realized.
As shown in fig. 1, the online sample collection system further includes a gas detection system 9, specifically, the gas detection system 9 includes a gas detection device 91, a water removal structure 92 and a second filter 93 connected in sequence, and the second filter 93 can be communicated with the reaction device 7 through a pipeline. The gas in the reaction device 7 can pass through the second filter 93 and the water removal structure 92 and then enter the gas detection device 91, so that the gas can be detected.
Further, the gas detection system 9 further includes a three-way valve 94, the three-way valve 94 has a first port, a second port and a third port, the first port is communicated with the water removal structure 92, the second port is communicated with the gas detection device 91, and the third port is an evacuation port. Through setting up three-way valve 94, can be when needs examine gas for first port and second port intercommunication need not to examine gas time, can make first port and third port intercommunication, carry out the evacuation to gas.
Optionally, in order to avoid that easily condensable components in the gas discharged from the reaction device 7 are condensed in the pipeline and adhere to particulate matters to cause pipeline blockage, the part of the sample injection pipeline 10 of the online sample collection system, which extends out of the reaction device 7, the pipeline between the first switching structure 4 and the second switching structure 5, and the pipeline between the second switching structure 5 and the sampling structure 2 are all wrapped with insulating layers. Furthermore, a heating structure can be arranged on each section of pipeline, and the heating structure can be a pipeline filled with high-temperature liquid or an electric heating structure; or each section of pipeline is set to be a double-layer structure, the inner layer is a pipeline for the circulation of solid materials, and high-temperature liquid can be arranged in the interlayer.
The reaction apparatus 7 is an experimental apparatus capable of performing a gas-solid two-phase reaction, and may be a metallic material or a non-metallic material (for example, quartz glass); the reaction can be carried out in a fixed bed, and can also be carried out in a fluidized bed state by externally connecting fluidizing gas; the method can be used for reactions occurring at normal temperature and reactions (including but not limited to catalysis, pyrolysis and gasification reactions) performed in a thermal state;
further, the reaction device 7 is provided with a heating structure (the specific structure is not labeled in the present invention). For example, a heating furnace may be provided outside the reaction apparatus 7.
The operation of the on-line sample collection system will be described in detail below.
1. Sampling structure 2 is connected with second switching structure 5 through the pipeline, makes collection bottle and evacuation system 6 intercommunication through second switching structure 5, closes the gas vent 21 of gathering the bottle, opens vacuum pump 61 afterwards, carries out the evacuation to the collection bottle, adjusts the vacuum of gathering the bottle through vacuum control valve 63, and the pressure in the bottle is in predetermineeing the pressure range until gathering, realizes gathering the regulation and control of bottle pressure.
2. The vacuum pump 61 is closed, after the pressure in the collection bottle is stable, the collection bottle is communicated with the first switching structure 4 through the second switching structure 5, meanwhile, the second switching structure 5 is communicated with the reaction device 7 through the first switching structure 4, solid materials in the reaction device 7 enter the collection bottle through the sampling pipeline 10, the first switching structure 4 and the second switching structure 5 under the action of the pressure difference between the reaction device 7 and the collection bottle, and the collection of solid material samples is realized.
3. After the sampling is accomplished, make collection bottle and evacuation system 6 intercommunication through second switch structure 5, carry inert gas in the pipeline between first switch structure 4 and the second switch structure 5 through first purge system 1 afterwards, inert gas enters into reaction unit 7 through first switch structure 4 and appearance pipeline 10, the realization is to the sweeping of remaining solid material in the pipeline between 8 and the first switch structure 4 and the appearance pipeline 10, open vacuum pump 61 simultaneously, again to the collection bottle evacuation, the gas that will enter into the collection bottle in by reaction unit 7 is taken out, prevent that solid material from continuing to take place the reaction.
4. And closing the vacuum pump 61, opening the exhaust port 21 of the collection bottle, communicating the collection bottle with the first purging system 1 through the second switching structure 5, communicating the reaction device 7 with the second purging system 3 through the first switching structure 4, and purging the sample introduction pipeline 10 again through the second purging system 3. Simultaneously, carry inert gas through first purge system 1 in to the pipeline between first switching structure 4 and the second switching structure 5, inert gas gets into through the second switching structure 5 and gathers in the bottle, realizes sweeping the pipeline between communicating structure 8 and the collection bottle, can also seal up the protection to the solid material in the collection bottle simultaneously.
5. The first purging system 1 is closed, the collection bottle is replaced, and the next sampling of the solid material is prepared. At this time, in order to prevent the solid material in the reaction device 7 from entering the sample introduction pipeline 10 under the action of the gas and reacting therein, so as to block the sample introduction pipeline 10, the second purging system 3 is preferably continuously opened during the sampling interval to purge the sample introduction pipeline 10.
When it is necessary to detect the gas in the reaction device 7, the first port and the second port of the three-way valve 94 are communicated, and the gas enters the gas detection device 91 after passing through the second filter 93 and the water removal structure 92. When the gas detection in the reaction device 7 is not required, the first port and the third port of the three-way valve 94 are made to communicate, and the gas in the reaction device 7 is evacuated.
In conclusion, the online sample collection system provided by the embodiment can vacuumize the sampling structure 2 through the vacuumizing system 6, on one hand, the solid materials in the reaction device 7 can enter the sampling structure 2 under the action of pressure difference, on the other hand, the gas entering the sampling structure 2 from the reaction device 7 can be pumped out, and the solid materials are prevented from continuously reacting. Through second purge system 3 and first purge system 1, can sweep completely the pipeline of this online sample system, first switching structure 4 and second switching structure 5, avoid remaining solid material in pipeline and the switching structure, and can also carry inert gas in to sampling structure 2 through first purge system 1 to protect the solid material in the sampling structure 2. This online sample collection system, compact structure can realize continuous sampling, and collection efficiency is high, and can avoid remaining solid material in pipeline and switching structure, guarantees the new freshness of gathering the sample and the accuracy of follow-up sample characterization result. In addition, the abrasion of residual particles in the switching structure to the switching structure when the switching structure is repeatedly used can be avoided, and the service life of the switching structure is prolonged.
The embodiment further provides an online sample collection method, which is applied to the online sample collection system, and specifically, the online sample collection method includes:
switching the second switching structure 5 to the sampling structure 2 to be communicated with the vacuumizing system 6, vacuumizing the sampling structure 2, adjusting the vacuum degree of the sampling structure 2 through a vacuum degree adjusting valve 63 until the internal pressure of the sampling structure 2 is within a preset pressure range, and stopping vacuumizing;
the reaction device 7 is communicated with the sampling structure 2 through a connecting pipeline by adjusting the first switching structure 4 and the second switching structure 5, and solid materials in the reaction device 7 enter the sampling structure 2 along the pipeline under the action of pressure difference between the reaction device 7 and the sampling structure 2;
adjusting the second switching structure 5 to enable the sampling structure 2 to be communicated with the vacuumizing system 6, vacuumizing the sampling structure 2 again to pump out reaction gas entering the sampling structure 2 from the reaction device 7, ensuring that the collected sample does not continuously react in the sampling structure 2, and meanwhile, conveying inert gas into a connecting pipeline between the reaction device 7 and the sampling structure 2 through the first purging system 1 to blow back part of the connecting pipeline between the connecting point of the first purging system 1 and the connecting pipeline and the reaction device 7, namely residual solid particles in the communicating structure 8 and the first switching structure 4 into the reaction device 7;
stopping vacuumizing the sampling structure 2, switching the first switching structure 4 to the second purging system 3 to be communicated with the reaction device 7, and purging the sample introduction pipeline 10 through the second purging system 3; and simultaneously, the second switching structure 5 is switched to the first blowing system 1 to be communicated with the sampling structure 2, the exhaust port 21 of the sampling structure 2 is opened, and inert gas is conveyed into the connecting pipeline between the reaction device 7 and the sampling structure 2 through the first blowing system 1, so that a part of the connecting pipeline between the connecting point of the first blowing system 1 and the connecting pipeline and the sampling structure 2, namely the solid particles remained in the connecting structure 8 and the second switching structure 5 are blown into the sampling structure 2 by the inert gas. And finishing the purging of the full sampling pipeline and the inert gas sealing of the collected sample.
The first purge system 1 is shut down, the sampling structure 2 is replaced, and the second purge system 3 is kept open. At this time, by keeping the second purging system 3 open, the solid material in the reaction device 7 can be prevented from entering the sample introduction line 10 under the action of the gas and reacting therein, so that the sample introduction line 10 is blocked. That is, the second purging system 3 is continuously turned on during the sampling pause to purge the sample line 10.
Further, the online sample collection method further comprises: the gas in the reaction device 7 is filtered and dehydrated and then enters the gas detection device 91. Specifically, the first port and the second port of the three-way valve 94 are made to communicate, and the gas in the reaction device 7 sequentially passes through the second filter 93, the water removal structure 92, and the three-way valve 94 and then enters the gas detection device 91.
The foregoing embodiments are merely illustrative of the principles and features of this invention, which is not limited to the above-described embodiments, but rather is susceptible to various changes and modifications without departing from the spirit and scope of the invention, which changes and modifications are within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (10)
1. An online sample collection system is characterized by comprising a first purging system (1) capable of conveying inert gas, a sampling structure (2), a second purging system (3), a first switching structure (4), a second switching structure (5) and a vacuum pumping system (6) which are sequentially connected through a pipeline, wherein the first purging system (1) is connected to the pipeline between the first switching structure (4) and the second switching structure (5), the sampling structure (2) is connected to the second switching structure (5), and the sampling structure (2) is provided with an exhaust port (21) capable of being opened and closed; the first switching structure (4) is connected with a sample introduction pipeline (10), the sample introduction pipeline (10) can extend into the solid material of the reaction device (7), and the second purging system (3) can convey gas of the same type as at least one gas in the reaction device (7);
the first switching structure (4) can selectively communicate the reaction device (7) with the second purging system (3) or the second switching structure (5), the second switching structure (5) can selectively communicate the sampling structure (2) with the first switching structure (4) or the vacuum-pumping system (6), and the vacuum-pumping system (6) is configured to evacuate the sampling structure (2) so that solid materials in the reaction device (7) enter the sampling structure (2) under the action of pressure difference.
2. The on-line sample collection system according to claim 1, wherein the first purge system (1) comprises a first gas storage tank (11), a first flow rate adjustment structure (12) and a first buffer tank (13) which are connected in sequence, the first gas storage tank (11) is filled with inert gas, and the first buffer tank (13) is connected to a pipeline between the first switching structure (4) and the second switching structure (5).
3. The on-line sample collection system according to claim 1, wherein the second purging system (3) comprises a second gas storage tank (31), a second flow regulating structure (32) and a second buffer tank (33) connected in sequence, the second gas storage tank (31) is filled with a gas of the same type as the at least one gas in the reaction device (7), and the second buffer tank (33) is connected to the first switching structure (4).
4. The on-line sample collection system according to claim 1, wherein the vacuum pumping system (6) comprises a vacuum pump (61), a first filter (62) and a vacuum degree regulating valve (63) which are connected in sequence, and the vacuum degree regulating valve (63) is connected to the second switching structure (5) through a pipeline.
5. The online sample collection system according to claim 1, further comprising a communication structure (8), wherein the communication structure (8) has a first port, a second port and a third port, each of which is connected in pairs, the first port is connected to the first purge system (1), the second port is connected to the first switching structure (4), and the third port is connected to the second switching structure (5).
6. The on-line sample collection system according to claim 1, further comprising a gas detection system (9), wherein the gas detection system (9) comprises a gas detection device (91), a water removal structure (92) and a second filter (93) which are connected in sequence, and the second filter (93) can be communicated with the reaction device (7) through a pipeline.
7. The on-line sample collection system according to claim 5 or 6, wherein the gas detection system (9) further comprises a three-way valve (94), the three-way valve (94) has a first port, a second port and a third port, the first port is communicated with the water removal structure (92), the second port is communicated with the gas detection device (91), and the third port is an evacuation port.
8. The on-line sample collection system of claim 1, wherein the portion of the sample introduction pipeline (10) extending out of the reaction device (7), the pipeline between the first switching structure (4) and the second switching structure (5), and the pipeline between the second switching structure (5) and the sampling structure (2) are wrapped with insulating layers.
9. An online sample collection method applied to the online sample collection system according to any one of claims 1 to 8, the online sample collection method comprising:
switching the second switching structure to a sampling structure to be communicated with a vacuumizing system, vacuumizing the sampling structure, adjusting the vacuum degree of the sampling structure through a vacuum degree adjusting valve until the pressure in the sampling structure is within a preset pressure range, and stopping vacuumizing;
the reaction device is communicated with the sampling structure through a connecting pipeline by adjusting the first switching structure and the second switching structure, and solid materials in the reaction device enter the sampling structure along the pipeline under the action of pressure difference between the reaction device and the sampling structure;
adjusting the second switching structure to communicate the sampling structure with the vacuum pumping system, and vacuumizing the sampling structure again to pump out the reaction gas entering the sampling structure from the reaction device, and simultaneously conveying inert gas into a connecting pipeline between the reaction device and the sampling structure through the first purging system to blow back residual solid particles in a part of the connecting pipeline between the connecting point of the first purging system and the connecting pipeline and the reaction device into the reaction device;
stopping vacuumizing the sampling structure, switching the first switching structure to a second purging system to be communicated with the reaction device, and purging the sample introduction pipeline through the second purging system; simultaneously, switching the second switching structure to a first blowing system to be communicated with the sampling structure, opening an exhaust port of the sampling structure, and conveying inert gas into a connecting pipeline between the reaction device and the sampling structure through the first blowing system so as to blow residual solid particles in a part of the connecting pipeline between the connecting point of the first blowing system and the connecting pipeline and the sampling structure into the sampling structure by using the inert gas;
and closing the first purging system, replacing the sampling structure and keeping the second purging system in an opening state.
10. The online sample collection method of claim 9, further comprising: the gas in the reaction device enters the gas detection device after being filtered and dewatered.
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