CN117451439A - System and method for collecting leakage of petrochemical water cooler - Google Patents
System and method for collecting leakage of petrochemical water cooler Download PDFInfo
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- CN117451439A CN117451439A CN202210843220.5A CN202210843220A CN117451439A CN 117451439 A CN117451439 A CN 117451439A CN 202210843220 A CN202210843220 A CN 202210843220A CN 117451439 A CN117451439 A CN 117451439A
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- OCKPCBLVNKHBMX-UHFFFAOYSA-N butylbenzene Chemical compound CCCCC1=CC=CC=C1 OCKPCBLVNKHBMX-UHFFFAOYSA-N 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
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- 239000003350 kerosene Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- QUEBYVKXYIKVSO-UHFFFAOYSA-N m-propyltoluene Chemical compound CCCC1=CC=CC(C)=C1 QUEBYVKXYIKVSO-UHFFFAOYSA-N 0.000 description 1
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- BWSNYLWZGNCWIH-UHFFFAOYSA-N naphthalene Chemical compound C1=CC=CC2=CC=CC=C21.C1=CC=CC2=CC=CC=C21 BWSNYLWZGNCWIH-UHFFFAOYSA-N 0.000 description 1
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- 229910052757 nitrogen Inorganic materials 0.000 description 1
- CXQXSVUQTKDNFP-UHFFFAOYSA-N octamethyltrisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)O[Si](C)(C)C CXQXSVUQTKDNFP-UHFFFAOYSA-N 0.000 description 1
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Classifications
-
- 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
- G01N1/22—Devices for withdrawing samples in the gaseous state
- G01N1/2202—Devices for withdrawing samples in the gaseous state involving separation of sample components during sampling
-
- 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
-
- 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
- G01N1/22—Devices for withdrawing samples in the gaseous state
Landscapes
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Biomedical Technology (AREA)
- Molecular Biology (AREA)
- Engineering & Computer Science (AREA)
- Hydrology & Water Resources (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
The invention relates to the technical field of leakage detection, and discloses a system and a method for collecting leakage matters of a petrochemical water cooler. The system comprises: the first collecting unit (100) is used for adsorbing liquid leakage and obtaining a first material flow, and the first collecting unit (100) is provided with a circulating water inlet and a first material flow outlet; the second collection unit (200) is used for collecting gaseous leakage and obtaining a second stream, a second stream outlet, a gaseous leakage outlet and a first stream inlet communicated with the first stream outlet are arranged on the second collection unit (200), a purge gas pipeline (300) is further arranged in the second collection unit (200), and the purge gas pipeline (300) is used for introducing purge gas to carry out gas stripping on the first stream. The acquisition system provided by the invention can acquire gaseous leakage matters and liquid leakage matters at the same time, so that fingerprint information of the leakage matters is more comprehensive.
Description
Technical Field
The invention relates to the technical field of leakage detection, in particular to a system and a method for collecting leakage matters of a petrochemical water cooler.
Background
The water-cooling heat exchanger (simply called water cooler) in the circulating water system of the refinery is loaded with heat exchange and cooling of most production devices of the refinery, and the water cooler may leak materials due to corrosion perforation and other reasons due to long-period running of the devices and poor crude oil quality.
Once the water cooler leaks, the circulating water quality is deteriorated, microorganisms are bred and a large amount of slime is bred, heat exchange equipment is blocked, other water cooling equipment in the system is corroded, even the device is stopped, and the damage to long-period stable operation of the petrochemical device is great.
Therefore, there is an urgent need to develop accurate and sensitive water cooler trace leakage detection technology, to discover leakage early and to cut off the leakage source, so as to avoid the continuous development and deterioration of leakage.
The water cooler involved in the whole circulating water system has various materials and complex components, not only comprises high-boiling-point oil products (such as diesel oil, kerosene and residual oil) but also comprises light products (such as methane and liquefied gas), and is used for monitoring different types of leakage matters in the circulating water, so that a plurality of analysis methods are needed to be combined.
CN206496874U discloses an on-line leakage monitor for a water cooler based on optical fibers, which uses optical fibers to isolate the influence of medium temperature in a pipeline on an optical device, adopts an ultraviolet fluorescence method, and adopts various compensation techniques such as built-in dark current, instrument culture diagram, sample temperature and the like, so that the accuracy of a detection result is greatly improved, but the device can only enrich and analyze liquid leakage in circulating water, and cannot detect gas leakage.
CN102279082a discloses an online monitoring method for leakage of petrochemical water cooler, which combines various detection technologies such as ultraviolet light splitting, ultraviolet fluorescence, optical fiber, infrared and gas detectors, so that potential safety hazards can be eliminated in time, time for checking leakage points during overhaul is saved, but larger manpower and material resource cost is consumed in the practical application process.
Therefore, a method capable of simultaneously collecting and detecting water leakage and liquid leakage of the circulating water of the water cooler is developed, and the method is convenient and economical to operate and has important significance in the petrochemical industry field.
Disclosure of Invention
The invention aims to solve the problem that in the prior art, gas leakage and liquid leakage cannot be collected and analyzed simultaneously in the circulating water leakage process of a water cooler.
In order to achieve the above object, a first aspect of the present invention provides an acquisition system for petrochemical water cooler leaks, the system being for acquiring liquid and gaseous leaks in petrochemical water cooler circulating water, comprising:
the first collecting unit is used for adsorbing liquid leakage and obtaining a first material flow, and a circulating water inlet and a first material flow outlet are formed in the first collecting unit;
the second collection unit is used for collecting gaseous leakage and obtaining second flow, a second flow outlet, a gaseous leakage outlet and a first flow inlet communicated with the first flow outlet are arranged on the second collection unit, a purge gas pipeline is further arranged in the second collection unit and used for introducing purge gas to carry out gas stripping on the first flow.
A second aspect of the present invention provides a method for collecting leakage from a petrochemical water cooler, the method being performed in a collection system according to the first aspect, comprising:
(1) Introducing circulating water into a first collecting unit to adsorb liquid leakage, so as to obtain a first material flow;
(2) Introducing the first material flow into a second acquisition unit in the presence of purge gas to carry out gas stripping treatment to obtain a second material flow and gaseous leakage;
in the circulating water, the liquid stateThe leakage is C 6-40 Alkane, C 6-40 Is C 6-40 Olefins and C of (2) 6-40 At least one of the aromatic hydrocarbons of (2) the gaseous leak is C 3 -C 5 Is a volatile hydrocarbon of (a).
The acquisition system for the leakage of the petrochemical water cooler can acquire the gaseous leakage and the liquid leakage at the same time, so that fingerprint information of the leakage is more comprehensive.
Particularly, the acquisition system provided by the invention has the advantages of accurate test result, convenience in carrying, simplicity and convenience in operation, and capability of greatly saving labor cost; and organic solvent is not needed in the extraction process, so that the method is green and economical.
Drawings
FIG. 1 is a schematic diagram of the system for collecting petrochemical water cooler leaks according to the present invention;
FIG. 2 is a graph of total ions of gaseous leaks in circulating water catalyzed oil and gas acquired by the method of the invention;
FIG. 3 is a graph showing total ion of liquid leakage in circulating water catalyzed oil gas obtained by the method of the invention;
FIG. 4 is a graph showing total ion of atmospheric and vacuum diesel and catalytic diesel in circulating water collected by the method of the present invention;
FIG. 5 is a graph showing total ion of catalytic oil gas, atmospheric and vacuum diesel and catalytic diesel in circulating water collected by a purge-trap method;
FIG. 6 is a graph showing total ion of catalytic oil gas, atmospheric and vacuum diesel and catalytic diesel in circulating water obtained by solid phase microextraction.
Description of the reference numerals
100. First acquisition unit 200, second acquisition unit
201. Accommodating tube I202 and accommodating tube II
300. Purge conduit 301 and bubble plate
400. Drying unit 500, filtering unit
600. Flowmeter 700 and gas collector
800. Inlet water regulating valve 900 and outlet water regulating valve
Detailed Description
The endpoints and any values of the ranges disclosed herein are not limited to the precise range or value, and are understood to encompass values approaching those ranges or values. For numerical ranges, one or more new numerical ranges may be found between the endpoints of each range, between the endpoint of each range and the individual point value, and between the individual point value, in combination with each other, and are to be considered as specifically disclosed herein.
The acquisition system and the acquisition method according to the present invention are described in detail below with reference to fig. 1 to 6 provided by the present invention.
As described above, the first aspect of the present invention provides a system for collecting liquid and gaseous leaks in petrochemical water cooler circulating water, comprising:
the first collecting unit 100 is used for adsorbing liquid leakage and obtaining a first material flow, and the first collecting unit 100 is provided with a circulating water inlet and a first material flow outlet;
the second collection unit 200, the second collection unit 200 is used for collecting the gaseous leakage and obtaining a second stream, and the second collection unit 200 is provided with a second stream outlet, a gaseous leakage outlet and a first stream inlet communicated with the first stream outlet, the inside of the second collection unit 200 is also provided with a purge gas pipeline 300, and the purge gas pipeline 300 is used for introducing purge gas to carry out gas stripping on the first stream.
In order to ensure that the circulating water is sufficiently purged without generating a relatively large air pressure, the distance between the bottom of the purge air pipe 300 and the bottom of the second collecting unit 200 is preferably 0.5-2cm, more preferably 1-2cm.
Preferably, the purge gas pipe 300 is at least one, more preferably 1.
Preferably, a bubbling board 301 for forming bubbles of the purge gas is further provided at the bottom of the purge gas pipe 300.
Preferably, a plurality of through holes (not shown in the drawings) are uniformly distributed on the frothing plate 301.
In order to increase the contact area of the purge gas with the water body and sufficiently purge hydrocarbons in the water, the average diameter of the through holes is preferably 10 to 100 μm.
Preferably, the purge gas is selected from inert gas and/or compressed air.
Preferably, the second collecting unit 200 includes a holding pipe I201 and a holding pipe II202 that are fixedly connected, the gaseous leakage outlet is disposed on the holding pipe I201, and the second outlet is disposed at the bottom of the holding pipe II 202.
In the invention, after the first material flow is introduced into the second collecting unit 200, the first material flow can continuously flow in the accommodating pipe II202 and is stripped under the action of the purge gas, and the accommodating pipe I201 can prevent the circulating water from splashing due to the stripping impact.
Preferably, the accommodating tube I201 is a spherical tube, and the accommodating tube II202 is a cylindrical tube.
In order to ensure that the second collection unit 200 can realize continuous large-volume sampling of volatile gaseous leakage in circulating water, the accommodating tube I201 and the accommodating tube II202 with different sizes can be designed according to the requirement, and the accommodating tube I201 in the invention has a volume of 0.05-0.5L, the accommodating tube II202 has a pipe diameter of 1-5cm, a volume of 0.01-0.5L and a height of 10-20cm.
More preferably, graduation marks are also provided on the accommodating tube II 202.
Preferably, the first collection unit 100 is a solid phase microextraction tube having a hollow tubular structure.
Preferably, the inner wall of the solid phase microextraction tube is provided with an adsorption material.
Preferably, the adsorption material is at least one selected from polydimethylsiloxane, polyacrylic acid, polyethylene glycol, carbon molecular sieve, carbon nanotube, graphene, aluminum oxide and divinylbenzene.
The invention has no special requirement on the size of the solid-phase microextraction tube, and the solid-phase microextraction tube with reasonable size can be designed according to the requirement, and the diameter of the tube inner cavity of the solid-phase microextraction tube is 1-5mm, preferably 3mm; the length is 2-5cm.
According to a particularly preferred embodiment of the present invention, the solid phase microextraction tube is a solid phase microextraction tube purchased from Qingdao Zhen company or a solid phase microextraction tube purchased from Sulpecco company, USA.
Preferably, the system further comprises:
a drying unit 400 for drying the gaseous leakage, the drying unit 400 being in communication with the gaseous leakage outlet and the interior of the drying unit 400 being filled with a desiccant.
Preferably, the drying agent is at least one selected from calcium chloride, activated alumina, molecular sieve and silica gel.
The kind of the drying unit 400 is not particularly limited in the present invention, and a dryer known in the art may be used.
Preferably, a gas collector 700 and/or a gas detector are provided at the gas outlet of the drying unit 400. The gas collector 700 is used to collect gaseous leaks and the gas detector is used to test the gas outlet concentration.
Preferably, the gas collector 700 is an air bag or a soda can.
Preferably, the system further comprises:
a filtering unit 500 for removing solid particles in the circulating water, the filtering unit 500;
the flowmeter 600 is disposed between the filtering unit 500 and the first collecting unit 100, and is used for testing the inflow rate of the circulating water.
The type of the filter unit 500 is not particularly limited, and a filter device known in the art may be used, and the filter unit 500 is exemplified by a pvc transparent Y-type filter device purchased from the company of samford, and the filter screen is 100 mesh.
A preferred embodiment of the collection system for petrochemical water cooler leaks of the present invention is described in detail below in conjunction with the configuration shown in fig. 1.
Circulating water from a refinery enters a collecting pipeline, a water inflow adjusting valve 800 adjusts the water inflow of the circulating water, the circulating water is conveyed to a filtering unit 500, and the filtering unit 500 removes solid slime particles in the circulating water; the flow rate of the inflow water of the circulating water is tested by a flowmeter 600, the circulating water is conveyed to the first collecting unit 100, and liquid leakage matters in the circulating water are adsorbed by an adsorption material in the first collecting unit 100 to obtain a first material flow; the first material flow is conveyed to the second collection unit 200, the first material flow continuously flows in the accommodating pipe II202 and is discharged from the second material outlet of the accommodating pipe II202 through the water outlet regulating valve 900, meanwhile, a purge gas is introduced into the purge gas pipeline 300, the purge gas forms uniform bubbles under the action of the bubble plate 301 to blow out and carry out gas stripping on the first material flow, the gaseous leakage obtained by gas stripping is conveyed to the drying unit 400 through the gaseous leakage outlet, and the dried gaseous leakage is conveyed to the gas collector 700.
The acquisition system for the leakage of the petrochemical water cooler provided by the invention also has the following specific advantages:
(1) The limitation that the existing sampling technology can only collect part of leakage matters in circulating water is broken through, and the volatile gaseous hydrocarbon and the liquid hydrocarbon which is insoluble in water can be collected, so that the fingerprint information of the leakage matters is more comprehensive.
(2) The collection system does not need to carry a large volume of water sample, is simple and convenient to operate, saves labor cost, does not need organic solvent in the extraction process, and is green and economical.
As previously mentioned, a second aspect of the present invention provides a method for collecting petrochemical water cooler leaks, the method being performed in a collection system according to the first aspect, comprising:
(1) Introducing circulating water into a first collecting unit to adsorb liquid leakage, so as to obtain a first material flow;
(2) Introducing the first material flow into a second acquisition unit in the presence of purge gas to carry out gas stripping treatment to obtain a second material flow and gaseous leakage;
in the circulating water, the liquid leakage is C 6-40 Alkane, C 6-40 Is C 6-40 Olefins and C of (2) 6-40 At least one of the aromatic hydrocarbons of (2) the gaseous leak is C 3 -C 5 Is a volatile hydrocarbon of (a).
Preferably, in the circulating water, the liquid leakage is selected from dodecane, tridecane, tetradecane, pentadecane, hexadecane, C 1 -C 4 At least one of an alkyl-substituted benzene, a substituted or unsubstituted naphthalene, and wherein the substituent is C 1 -C 3 Is a hydrocarbon group.
Preferably, in the circulating water, the gaseous leak is at least one selected from propylene, isobutane, n-butane, 2-butene, 2-methylbutane, n-pentane.
Preferably, in the step (1), the flow rate of the circulating water is 0.1-1L/min.
The present invention has no particular requirement for the operation of the adsorption treatment in step (1), and only needs to meet the requirement of the present invention, and the adsorption treatment is completed after circulating water continuously flows until 5-10L of water flows at room temperature, for example.
Preferably, in the step (2), the flow rate of the purge gas is 50-100mL/min.
The invention will be described in detail below by way of examples.
In the following examples, the circulating water adopted is collected from a circulating water inlet pipeline of a catalytic cracking device of a refinery in 2021 month 12, the water quality is clear and transparent, no petroleum hydrocarbon is detected by adopting a gas chromatograph-mass spectrometer, the circulating water is taken as blank circulating water, and 100mg/L of catalytic oil gas, 100mg/L of atmospheric and vacuum diesel oil and 100mg/L of catalytic diesel oil are respectively added into the circulating water;
the first acquisition unit: the solid phase microextraction tube has a cavity diameter of 3mm and a length of 3cm, the adsorption material of the inner wall is polydimethylsiloxane, and the thickness of the adsorption material is 60 mu m, and the adsorption material is purchased from Qingdao Zhen company;
in the following examples, 1 purge pipe is used;
the accommodating tube I is a spherical tube, the volume is 0.1L, and the glass material is used for accommodating the glass material;
the accommodating tube II is a cylindrical glass tube, the volume is 0.1L, and the tube diameter is 3cm;
the dryer is a spherical drying tube, and the drying agent is silica gel;
in the following examples, the purge gas is nitrogen unless otherwise specified;
gas collector: the air bag has a volume of 1L and is purchased from Dalian sea technologies limited company;
thermal desorption tube: 1/4 inch in diameter and 3.5 inches long, model 495094, available from MARKES, UK;
in the following examples, the model of the gas chromatograph-mass spectrometer is 8890/5977B, available from Agilent corporation, unless otherwise stated;
wherein, the chromatographic conditions are as follows: HP-PONA capillary chromatographic column (50 m.times.0.2 mm.times.0.25 μm); the temperature of the sample inlet is 260 ℃, the split ratio is 5:1, and the temperature of the column is programmed to rise: the initial column temperature was 40℃and maintained for 5min, and the temperature was raised to 320℃at a rate of 5℃per min. The mass spectrum conditions are as follows: an EI source, electron energy of 70eV, ion source temperature of 230 ℃; the MS quadrupole is 150 ℃; the transmission line temperature is: 280 ℃; the acquisition mode is as follows: full scanning; the scanning quality range is as follows: (5-300) amu.
Example 1
The structure (or process) shown in fig. 1 is used to collect leaks in petrochemical water coolers.
Circulating water from a refinery enters a collecting pipeline, a water inflow adjusting valve 800 adjusts the water inflow of the circulating water, the circulating water is conveyed to a filtering unit 500, and the filtering unit 500 removes solid slime particles in the circulating water; the method comprises the steps of testing the inflow rate of circulating water by using a flowmeter 600, wherein the inflow rate is 0.5L/min, the circulating water is conveyed to a first acquisition unit 100, and liquid leakage matters in the circulating water are adsorbed by an adsorption material in the first acquisition unit 100 to obtain a first material flow; the first material flow is sent to the second collection unit 200, the first material flow continuously flows in the accommodating pipe II202 and is discharged from the second material outlet of the accommodating pipe II202 through the water outlet regulating valve 900, meanwhile, a purge gas is introduced into the purge gas pipe 300, the flow rate of the purge gas is 0.05L/min, the purge gas forms uniform bubbles under the action of the bubble plate 301 (the average diameter of the through holes on the bubble plate is 50 μm) to blow out and carry out stripping on the first material flow, the gaseous leakage obtained by stripping is sent to the drying unit 400 through the gaseous leakage outlet, and the dried gaseous leakage is sent to the gas collector 700. The sampling time is recorded and the timing is started from the opening of the water inlet regulating valve 800.
The calculation formula of the water sample volume is as follows: v = μt;
v represents the volume of the water sample, L;
mu represents the water inflow flow of the circulating water tested by the flowmeter 600, L/min;
t represents sampling time, min;
in this example t is 15min and the water sample volume is 0.5L/min x 15min = 7.5L.
The liquid leakage adsorbed in the first collecting unit 100 and the gaseous leakage in the gas collector 700 were analyzed by chromatography-mass spectrometry, respectively, and the specific analysis results are shown in tables 1 and 2.
The preparation method of the liquid leakage sample comprises the following steps: after the sampling is finished, the solid-phase microextraction tube is taken down and put into a thermal desorption tube; then the thermal desorption tube is inserted into a thermal desorption assembly of a thermal desorption instrument and screwed; starting a thermal desorption instrument (model is Centri, purchased from Markes company), heating to 250 ℃ for 2min, and maintaining the temperature for thermal desorption for 5min; and (5) starting a gas chromatography-mass spectrometry combined analyzer for analysis.
The invention also provides an example of total ion diagrams of gaseous leakage matters and liquid leakage matters in the circulating water acquired by the method, and the total ion diagrams are respectively shown in fig. 2-4.
Wherein, fig. 2 is a total ion diagram of gaseous leakage in circulating water catalytic oil gas acquired by the method of the invention, fig. 3 is a total ion diagram of liquid leakage in circulating water catalytic oil gas acquired by the method of the invention, fig. 4 is a total ion diagram of atmospheric and vacuum diesel oil and catalytic diesel oil in circulating water acquired by the method of the invention, fig. 4a is a total ion diagram of atmospheric and vacuum diesel oil in circulating water acquired by the method of the invention, and fig. 4b is a total ion diagram of catalytic diesel oil in circulating water acquired by the method of the invention.
As can be seen from FIGS. 2 to 4, the method provided by the invention can be used for simultaneously collecting the total number of carbon atoms C 3 -C 5 The sum of the volatile hydrocarbons and the carbon atoms of (C) 6 The above water-insoluble liquid hydrocarbon.
Comparative example 1
The leakage in the circulating water is collected by adopting a purging and trapping method, and is analyzed by adopting a chromatographic-mass spectrometry, and the specific analysis result is shown in fig. 5.
The purging and trapping method is carried out on a commercial instrument ATOMX solid-liquid phase purging and trapping concentration sample injector, a sample solution is poured into a 40mL sample injection bottle, the bottle is sealed after overflow, and an automatic sample injector takes 5mL of water sample for purging and trapping treatment.
The process parameters in the process of purging and trapping are as follows: the purge gas was helium (purity 99.999%), the purge tube volume was 5mL, the purge temperature was room temperature, the purge flow rate was 40mL/min, the purge time was 10min, the pre-desorption temperature was 180 ℃, the pre-desorption time was 1min, the desorption temperature was 190 ℃, the desorption time was 2min, the bake temperature was 200 ℃, the bake time was 6min, and the transmission line temperature was 150 ℃.
Fig. 5a is a total ion diagram of catalytic oil gas in circulating water acquired by adopting a purge-trap method, fig. 5b is a total ion diagram of atmospheric and vacuum diesel oil in circulating water acquired by adopting a purge-trap method, and fig. 5c is a total ion diagram of catalytic diesel oil in circulating water acquired by adopting a purge-trap method.
As can be seen from fig. 5, the purge-and-trap method can be used for detecting light hydrocarbon components in the oil gas, but for heavy oil products such as atmospheric and vacuum diesel oil and relatively light catalytic light diesel oil, the detected components are less, and the result shows that the purge-and-trap method is suitable for analyzing light oil leakage in water and is not suitable for analyzing oil leakage with more heavy components.
Comparative example 2
The leakage in the circulating water is collected by adopting a solid-phase microextraction method, and is analyzed by adopting a chromatographic-mass spectrometry method, and the specific analysis result is shown in figure 6.
The solid phase micro extraction is carried out on a CTC automatic device, a Solid Phase Micro Extraction (SPME) mode is selected, 19mL of water sample is taken and added into a 20mL headspace bottle, a solid phase probe is pricked into the water sample, after the oscillation extraction is carried out at 40 ℃ for 40min, the probe is pricked into a chromatographic sample inlet, the desorption is carried out at 260 ℃ for 3min, the desorption gas enters a gas chromatography-mass spectrometry combined analyzer for analysis, the carrier gas is helium (the purity is 99.999%), the SPME probe is purchased from Sulpecco company, the coating material is PDMS, the coating thickness is 100 mu m, and the probe size is 24ga.
Fig. 6a is a total ion diagram of catalytic oil gas in circulating water, which is acquired by a solid-phase microextraction method, fig. 6b is a total ion diagram of atmospheric and vacuum diesel oil in circulating water, which is acquired by a solid-phase microextraction method, and fig. 6c is a total ion diagram of catalytic diesel oil in circulating water, which is acquired by a solid-phase microextraction method.
As can be seen from fig. 6, the accuracy of the test results by the solid-phase microextraction method is low, and the collected leakage is not comprehensive enough.
Table 1: analysis result of catalytic oil gas liquid leakage in circulating water
| Sequence number | Retention time | Molecular formula | CAS number | Names of Compounds | Peak area percent/% |
| 1 | 15.264 | C 8 H 10 | 100-41-4 | Ethylbenzene (ethylbenzene) | 26.7 |
| 2 | 15.630 | C 8 H 10 | 108-38-3 | Xylene (P) | 100 |
| 3 | 16.530 | C 8 H 10 | 106-42-3 | Xylene (P) | 42.54 |
| 4 | 18.835 | C 9 H 12 | 103-65-1 | Propyl benzene | 5.03 |
| 5 | 19.111 | C 9 H 12 | 611-14-3 | Cumene (isopropyl benzene) | 24.31 |
| 6 | 19.183 | C 9 H 12 | 622-96-8 | 1-ethyl-4-methyl-benzene | 9.59 |
| 7 | 19.373 | C 9 H 12 | 108-67-8 | Trimethylbenzene | 10.86 |
| 8 | 20.342 | C 9 H 12 | 526-73-8 | Trimethylbenzene | 42.1 |
| 9 | 21.802 | C 9 H 12 | 300-57-2 | 2-propenylbenzene | 10.73 |
| 10 | 22.021 | C 9 H 8 | 2327-99-3 | Styrene | 1.93 |
| 11 | 22.33 | C 10 H 14 | 1074-43-7 | 3-methyl-propylbenzene | 3.28 |
| 12 | 22.54 | C 10 H 14 | 874-41-9 | 2, 4-dimethyl-ethylbenzene | 5.14 |
| 13 | 22.912 | C 10 H 14 | 135-98-8 | 1-methylpropyl-benzene | 1.5 |
| 14 | 23.226 | C 10 H 14 | 1758-88-9 | 2, 5-dimethyl-ethylbenzene | 3.47 |
| 15 | 23.507 | C 10 H 14 | 934-74-7 | 3, 5-dimethyl-ethylbenzene | 5.68 |
| 16 | 23.597 | C 10 H 12 | 767-58-8 | 1-methyl-indane | 3.14 |
| 17 | 24.735 | C 10 H 14 | 95-93-2 | 1,2,3, 5-tetramethyl-benzene | 3.91 |
| 18 | 25.35 | C 10 H 12 | 824-22-6 | 2-ethyl-1, 3-dimethylbenzene | 4.45 |
| 19 | 25.702 | C 10 H 12 | 1587-04-8 | 1-methyl-2- (2-propenyl) -benzene | 6.36 |
| 20 | 25.797 | C 10 H 14 | 95-93-2 | 1,2,4, 5-tetramethyl-benzene | 4.36 |
| 21 | 26.745 | C 10 H 8 | 91-20-3 | Naphthalene (naphthalene) | 24.03 |
| 22 | 30.136 | C 11 H 10 | 91-57-6 | 2-methylnaphthalene | 3.02 |
| 23 | 30.850 | C 11 H 10 | 90-12-0 | 1-methylnaphthalene | 2.1 |
Table 2: analysis result of atmospheric and vacuum diesel oil liquid leakage in circulating water
As can be seen from the results in tables 1 and 2, the method provided by the invention has more accurate test results and more comprehensive fingerprint information of the obtained leakage.
The preferred embodiments of the present invention have been described in detail above, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, a number of simple variants of the technical solution of the invention are possible, including combinations of the individual technical features in any other suitable way, which simple variants and combinations should likewise be regarded as being disclosed by the invention, all falling within the scope of protection of the invention.
Claims (13)
1. The utility model provides a collection system for petrochemical water cooler leakage thing, its characterized in that, this system is used for gathering petrochemical water cooler circulating water's liquid leakage thing and gaseous leakage thing, contains:
the first collecting unit (100), the first collecting unit (100) is used for absorbing liquid leakage and obtaining a first material flow, and the first collecting unit (100) is provided with a circulating water inlet and a first material flow outlet;
the second collection unit (200), second collection unit (200) are used for gathering gaseous state leakage thing and obtain the second stream, just be provided with second stream outlet, gaseous state leakage thing export on second collection unit (200), with the first commodity circulation entry of first commodity circulation export intercommunication, the inside of second collection unit (200) still is provided with sweep gas pipeline (300), sweep gas pipeline (300) are used for introducing the sweep gas in order to carry out the stripping to first commodity circulation.
2. The acquisition system according to claim 1, wherein the distance between the bottom of the purge gas line (300) and the bottom of the second acquisition unit (200) is 0.5-2cm, preferably 1-2cm.
3. The acquisition system according to claim 1 or 2, wherein the purge gas lines (300) are at least one, preferably 1-3.
4. A collection system according to any one of claims 1-3, wherein the bottom of the purge gas line (300) is further provided with a frothing plate (301) for bubbling the purge gas;
preferably, a plurality of through holes are uniformly distributed on the foaming plate (301);
preferably, the average diameter of the through holes is 10-100 μm.
5. The acquisition system according to any one of claims 1-4, wherein the purge gas is selected from inert gas and/or compressed air.
6. The collecting system according to any one of claims 1-5, wherein the second collecting unit (200) comprises a fixedly connected containment tube I (201) and a containment tube II (202), the gaseous leakage outlet being arranged on the containment tube I (201) and the second stream outlet being arranged at the bottom of the containment tube II (202).
7. The collection system according to any one of claims 1-6, wherein the first collection unit (100) is a solid phase microextraction tube having a hollow tubular structure;
preferably, the inner wall of the solid-phase microextraction tube is provided with an adsorption material;
preferably, the adsorption material is at least one selected from polydimethylsiloxane, polyacrylic acid, polyethylene glycol, carbon molecular sieve, carbon nanotube, graphene, aluminum oxide and divinylbenzene.
8. The acquisition system according to any one of claims 1-7, wherein the system further comprises:
-a drying unit (400) for drying the gaseous leakage, the drying unit (400) being in communication with the gaseous leakage outlet and the interior of the drying unit (400) being filled with a desiccant;
preferably, the drying agent is at least one selected from calcium chloride, activated alumina, molecular sieve and silica gel.
9. The acquisition system according to any one of claims 1-8, wherein the system further comprises:
-a filtration unit (500), the filtration unit (500) being adapted to remove solid particles from the circulating water;
the flowmeter (600) is arranged between the filtering unit (500) and the first collecting unit (100) and is used for testing the inflow flow of circulating water.
10. A method for collecting petrochemical water cooler leaks, the method being carried out in a collection system according to any one of claims 1 to 9, comprising:
(1) Introducing circulating water into a first collecting unit to adsorb liquid leakage, so as to obtain a first material flow;
(2) Introducing the first material flow into a second acquisition unit in the presence of purge gas to carry out gas stripping treatment to obtain a second material flow and gaseous leakage;
in the circulating water, the liquid leakage is C 6-40 Alkane, C 6-40 Is C 6-40 Olefins and C of (2) 6-40 At least one of the aromatic hydrocarbons of (2) the gaseous leak is C 3 -C 5 Is a volatile hydrocarbon of (a).
11. The method of claim 10, wherein in the circulating water the liquid leak is selected from the group consisting of dodecane, tridecane, tetradecane, pentadecane, hexadecane, and C 1 -C 4 At least one of an alkyl-substituted benzene, a substituted or unsubstituted naphthalene, and wherein the substituent is C 1 -C 3 Alkyl of (a);
preferably, in the circulating water, the gaseous leak is at least one selected from propylene, isobutane, n-butane, 2-butene, 2-methylbutane, n-pentane.
12. The collecting method according to claim 10 or 11, wherein in step (1), the flow rate of the circulating water is 0.1-1L/min.
13. The acquisition method according to any one of claims 10 to 12, wherein, in the step (2), the flow rate of the purge gas is 50 to 100mL/min.
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