1. A fluoride leak detection apparatus characterized in that: comprises a collecting cover (1), a separating device (2) and a detecting device (3);

a collecting port (5) for collecting leaked gas and an output port (7) communicated with the separating device (2) are arranged on the collecting cover (1);

the separation device (2) is configured to separate the leakage gas into fluoride gas and output the fluoride gas; the detection device (3) is communicated with the output end of the separation device (2) and is used for detecting the concentration data of the fluoride gas.

2. The fluoride leak detection apparatus of claim 1, wherein: an input port (6) is also arranged on the collecting cover (1), and the input port (6) is communicated with a gas carrying bottle (4); inert gas is arranged in the gas carrying bottle (4);

a first flow controller (8) is arranged between the input port (6) and the gas carrying bottle (4);

a second flow controller (9) is arranged between the output port (7) and the separating device (2).

3. The fluoride leak detection apparatus of claim 2, wherein: the input port (6) is also communicated with an input device (10) for inputting standard gas, and the standard gas component is consistent with the leakage gas component.

4. The fluoride leak detection apparatus of claim 3, wherein: an air pump (12) is arranged between the output port (7) and the second flow controller (9), the output end of the air pump (12) is also communicated with an exhaust pipeline (13), and an exhaust valve (14) is arranged in the exhaust pipeline (13).

5. The fluoride leak detection apparatus of claim 2, wherein: the separation device (2) comprises a plurality of detection channels (15) which are arranged in parallel; one end of the detection channel (15) is communicated with the second flow controller (9), and the other end of the detection channel is communicated with the detection device (3) through a selective valve (16);

and a detection valve (17) and a separation column (18) for separating the leaked gas are arranged in each detection channel (15).

6. The fluoride leak detection apparatus of claim 2, wherein: the gas carrying bottle (4) is communicated with the input port (6) through an input pipeline (19); the first flow controller (8) is arranged in the input pipe (19); an input valve (20) is arranged in the input pipeline (19) and close to one end of the input port (6).

7. The fluoride leak detection apparatus of claim 2, wherein: the output port (7) is communicated with the separating device (2) through an output pipeline (21), and the second flow controller (9) is arranged in the output pipeline (21).

8. The fluoride leak detection apparatus of any of claims 1 to 7, wherein: the collecting port (5) is arranged at the bottom of the collecting cover (1); the collecting cover (1) is provided with a hose clamp (22); a sealing ring (27) is arranged at the bottom of the collecting cover (1); a fan (11) is arranged in the collecting cover (1).

9. A detection method using the fluoride leak detection apparatus of claim 4, characterized in that: the method comprises the following steps:

and (3) detecting leakage: mounting the collecting hood (1) on a production pipeline; accumulated t₁Time, starting the separation device (2) and the detection device (3); when the concentration of the gas output by the detection device (3) is judged to be greater than a set value, the production pipeline is leaked;

obtaining a concentration peak area S1 of the fluoride gas: when the concentration peak output by the detection device (3) is judged to be complete, the concentration peak area S output by the detection device (3) is directly obtained₁(ii) a When the concentration peak shape output by the detection device (3) is judged to be peak clipping, the gas carrying bottle (4) is opened and the flow Q of the first flow controller (8) is adjusted₁With the flow Q of the second flow controller (9)₂Obtaining said detectionConcentration peak area S output from device (3)₁；

Injecting standard gas: injecting a volume V into the collecting cover (1) through the input device (10)₂Standard gas of (2), cumulative t₂Time, obtaining the concentration peak area S output by the detection device (3)₂；

Calculating the leakage rate:

wherein q is₁For the concentration of fluoride gas in the leaking gas, q₂Is the fluoride gas concentration in the standard gas.

10. The detection method using a fluoride leak detection apparatus according to claim 9, characterized in that: the method also comprises the following steps before detecting the leaked gas:

opening the air suction pump (12) and an exhaust valve (14) to suck the air pressure in the collecting cover (1) to negative pressure;

the air pump (12) is closed, the gas carrying bottle (4) is opened, the air pressure in the collecting cover (1) is filled to the standard atmospheric pressure, and then the air is continuously filled for 3-5 min; and closing the gas carrying bottle (4) and the exhaust valve (14).

Background

In the long-term uninterrupted operation process of the production device of the organic oxide, the raw material or product is frequently leaked due to the influences of high temperature, high pressure, corrosion and the like; most of the organic fluorides are toxic, and meanwhile, the organic fluorides have flammable and explosive properties, so that serious accidents can be caused once leakage occurs;

in the prior art, fluoride production devices are generally subjected to pre-delivery detection or on-line detection; mass spectrum leak detection is mostly adopted for pre-delivery detection, which has high sensitivity, but if production devices in a production state need to be detected, local production halt needs to be carried out, which inevitably causes a great amount of economic loss; the on-line detection mostly adopts a pressure change method and a bubble detection method; although the pressure variation method does not need production halt detection, the pressure variation method can only detect the total leakage rate of the equipment and cannot realize leakage positioning, and meanwhile, the equipment pressure is always in a fluctuation state in the production process, so that the pressure variation method can only detect large leakage and cannot realize micro-leakage detection; the bubble detection method needs to spray bubble liquid (generally soap liquid) on a leakage risk part on equipment, the method needs operators to carefully observe the change condition of bubbles according to experience, and the detection sensitivity has more subjective factors; meanwhile, the bubble liquid and the equipment are easy to generate chemical corrosion and electrochemical corrosion, and the safety of the equipment is affected.

Disclosure of Invention

In view of the above-mentioned drawbacks and deficiencies of the prior art, it would be desirable to provide a fluoride leak detection apparatus and method that does not require any downtime for detection and that does not damage the production equipment.

In a first aspect, the present application provides a fluoride leakage detection apparatus comprising a collection enclosure, a separation device, and a detection device;

the collecting cover is provided with a collecting port for collecting leaked gas and an output port communicated with the separating device;

the separation device is configured to separate the leakage gas into fluoride gas and output the fluoride gas; the detection device is communicated with the output end of the separation device and is used for detecting the concentration data of the fluoride gas.

In a preferred embodiment of the collecting hood, the collecting hood is further provided with an input port, and the input port is communicated with a gas carrying bottle; inert gas is arranged in the gas carrying bottle;

a first flow controller is arranged between the input port and the gas carrying bottle;

and a second flow controller is arranged between the output port and the separating device.

According to the technical scheme provided by the embodiment of the application, the input port is also communicated with an input device for inputting standard gas, and the standard gas component is consistent with the leaked gas component.

According to the technical scheme provided by the embodiment of the application, the delivery outlet with be equipped with the aspiration pump between the second flow controller, the aspiration pump output still communicates there is the exhaust duct, be equipped with the exhaust valve in the exhaust duct.

According to the technical scheme provided by the embodiment of the application, the separation device comprises a plurality of detection channels which are arranged in parallel; one end of the detection channel is communicated with the second flow controller, and the other end of the detection channel is communicated with the detection device through a gate valve; and a detection valve and a separation column for separating the leaked gas are arranged in each detection channel.

According to the technical scheme provided by the embodiment of the application, the gas carrying bottle is communicated with the input port through an input pipeline; the first flow controller is disposed within the input pipe; an input valve is arranged in the input pipeline and close to one end of the input port.

According to the technical scheme provided by the embodiment of the application, the output port is communicated with the separation device through an output pipeline, and the second flow controller is arranged in the output pipeline.

According to the technical scheme provided by the embodiment of the application, the collecting port is arranged at the bottom of the collecting cover; the collecting cover is provided with a hose clamp; a sealing ring is arranged at the bottom of the collecting cover; a fan is installed in the collecting cover.

In a second aspect, the present application provides a detection method using the fluoride leak detection apparatus as described above, comprising the steps of:

and (3) detecting leakage: mounting the collection hood on a production pipeline; accumulated t₁Time, starting the separating device and the detecting device; when the concentration of the gas output by the detection device is judged to be greater than a set value, the production pipeline is leaked;

obtaining the concentration peak area S of the fluoride gas₁: when the concentration peak output by the detection device is judged to be complete, the concentration peak area S output by the detection device is directly obtained₁(ii) a When the concentration peak shape output by the detection device is judged to be peak clipping, the gas carrying bottle is opened and the flow Q of the first flow controller is adjusted₁With said second flow controller flow rate Q₂Obtaining the concentration peak area S output by the detection device₁；

Injecting standard gas: injecting a volume V into the collecting cover through the standard gas input device₂Standard gas of (2), cumulative t₂Time, obtaining the concentration peak area S output by the detection device₂；

Calculating the leakage rate:

wherein q is₁For the concentration of fluoride gas in the leaking gas, q₂Is the fluoride gas concentration in the standard gas.

According to the technical scheme provided by the embodiment of the application, the method further comprises the following steps before the leakage gas is detected:

opening the air pump and the exhaust valve to pump the air pressure in the collecting cover to negative pressure;

closing the air pump, opening the gas carrying bottle, filling the air pressure in the collecting cover to the standard atmospheric pressure, and then continuing to fill inert gas for 3-5 min; and closing the gas carrying cylinder and the exhaust valve.

The beneficial effect of this application lies in: when in use, the collecting cover can be detachably and quickly arranged at the position to be detected on the production pipeline; after accumulating for a period of time, starting the separation device and the detection device; when the position to be detected leaks, the leaked gas leaks into the collecting cover and is accumulated continuously, the fluoride gas is separated by the separating device, and then the data of the fluoride gas leakage at the position can be detected and calculated by the detecting device.

The application provides a pair of fluoride leak testing equipment can carry out the qualitative and quantitative analysis of little leakage gas to each position on the production pipeline under the state of not shutting down, and the testing process can not cause production equipment to cause the harm, can not receive the interference of fluctuation pressure in the production pipeline, and the testing result is comparatively accurate.

Drawings

Other features, objects and advantages of the present application will become more apparent upon reading of the following detailed description of non-limiting embodiments thereof, made with reference to the accompanying drawings in which:

FIG. 1 is a schematic view of a fluoride leak detection apparatus provided herein;

FIG. 2 is a schematic view of the installation structure of the collecting cover 1 shown in FIG. 1;

FIG. 3 is a flow chart of a method of detection of the fluoride leak detection apparatus of FIG. 1;

FIG. 4 is a schematic diagram showing the peak clipping of the concentration peak pattern output from the detection apparatus 3 shown in FIG. 1;

fig. 5 is a schematic diagram of the concentration peak profile output by the monitoring device 3 shown in fig. 1 when complete.

Reference numbers in the figures:

1. a collection hood; 2. a separation device; 3. a detection device; 4. a gas-carrying cylinder; 5. a collection port; 6. an input port; 7. an output port; 8. a first flow controller; 9. a second flow controller; 10. a standard gas input device; 11. a fan; 12. an air pump; 13. an exhaust duct; 14. an exhaust valve; 15. a detection channel; 16. a gate valve; 17. a check valve; 18. a separation column; 19. an input pipe; 20. an input valve; 21. an output pipe; 22. a hose clamp; 23. a first start-up valve; 24. a second actuation valve; 25. a lug is tied; 26. producing a pipeline; 27. and (5) sealing rings.

Detailed Description

The present application will be described in further detail with reference to the following drawings and examples. It is to be understood that the specific embodiments described herein are merely illustrative of the relevant invention and not restrictive of the invention. It should be noted that, for convenience of description, only the portions related to the present invention are shown in the drawings.

It should be noted that the embodiments and features of the embodiments in the present application may be combined with each other without conflict. The present application will be described in detail below with reference to the embodiments with reference to the attached drawings.

Example 1

Please refer to fig. 1, which is a schematic diagram of a fluoride leakage detecting apparatus provided in the present application, including a collecting cover 1, a separating device 2 and a detecting device 3;

the collecting cover 1 is provided with a collecting port 5 for collecting leaked gas and an output port 7 communicated with the separating device 2;

the separation device 2 is configured to separate the leakage gas into fluoride gas and output the fluoride gas; the detection device 3 is communicated with the output end of the separation device 2 and is used for detecting the concentration data of the fluoride gas.

Specifically, the collecting cover 1 is detachably mounted on the production pipeline, and the collecting port 5 corresponds to a position to be measured on the production pipeline 26.

In particular, the separation device 2 is configured to separate the leakage gas from a fluoride gas. The detection device 3 is used for detecting the concentration peak area of the fluoride gas.

The working principle is as follows: when in use, the collecting cover 1 is detachably and quickly arranged at the position to be detected on the production pipeline; after accumulating for a period of time, opening the separation device 2 and the detection device 3; when the position to be detected leaks, the leaked gas leaks into the collecting cover 1 and is accumulated continuously, the fluoride gas is separated by the separating device 2, and the data of the fluoride gas leakage at the position can be detected and calculated by the detecting device 3. Wherein the concentration data comprises concentration peak area. The obtained concentration peak area is used to calculate the leak rate at that location.

The application provides a pair of fluoride leak testing equipment can carry out the qualitative and quantitative analysis of little leakage gas to each position on the production pipeline under the state of not shutting down, and the testing process can not cause the harm to production equipment, can not receive the interference of fluctuation pressure in the production pipeline, and the testing result is comparatively accurate.

In a preferred embodiment of the collecting cover 1, an input port 6 is further arranged on the collecting cover 1, and the input port 6 is communicated with a gas carrying bottle 4; inert gas is arranged in the gas carrying bottle 4;

a first flow controller 8 is arranged between the input port 6 and the gas carrying bottle 4;

a second flow controller 9 is arranged between the output port 7 and the separating device 2.

Specifically, the inert gas is helium;

the working principle is as follows: when the leakage of the position to be detected of the production pipeline is large, the concentration of the gas leaked into the collecting cover 1 is large, the peak area of the concentration of the fluoride gas detected by the detection device 3 is prone to peak clipping, the gas carrying bottle 4 can be opened when the peak clipping occurs, the flow ratio of the first flow controller 8 and the second flow controller 9 is adjusted at the same time, the concentration of the gas in the collecting cover 1 is reduced, a complete peak shape is obtained, and then the leakage rate of the position is obtained.

As will be known by those skilled in the art, the term "peak clipping phenomenon" refers to a phenomenon that the concentration of the gas to be measured exceeds the detection limit of the device, i.e., the peak clipping phenomenon occurs in the output concentration peak waveform. The full gas concentration peak profile is shown in fig. 4, and the peak profile of the peak clipping gas concentration peak profile is shown in fig. 5.

Preferably, the input port 6 is also connected to an input device 10 for inputting a standard gas, the standard gas composition being identical to the leaking gas composition.

The method for obtaining the leakage rate comprises the following steps:

and (3) detecting leakage: mounting the collecting hood 1 on a production pipe 26; tired ofProduct t₁Time, the separation device 2 and the detection device 3 are started; when the concentration of the gas output by the detection device 3 is judged to be greater than a set value, the production pipeline 26 has leakage;

specifically, t is accumulated₁The time can make the leakage gas in the collection cover 1 accumulate to a certain concentration, which is convenient for detection.

Obtaining the concentration peak area S1 of fluoride gas: when the concentration peak output by the detection device 3 is judged to be complete, directly obtaining the concentration peak area S1 output by the detection device 3; when the concentration peak shape output by the detection device 3 is judged to be peak clipping, the gas carrying bottle 4 is opened and the flow Q of the first flow controller 8 is adjusted₁With said second flow controller 9 flow rate Q₂The concentration peak area S1 output by the detection device 3 is obtained again;

injecting standard gas: injecting a volume V into the collecting cover 1 through the input device 10₂Standard gas of (2), cumulative t₂Time, obtaining a concentration peak area S2 output by the detection device 3;

calculating the leakage rate:

wherein q is₁For leakage gas concentration, q₂Is the standard gas concentration.

In the process, because the standard gas and the leakage gas are tested by the same detection device 3 for the concentration peak area, the measurement errors of different environments and different devices are avoided; the qualitative and quantitative analysis of micro leakage of each position to be measured of the production pipeline can be realized without stopping the production pipeline.

In a preferred embodiment of the output port 7, an air suction pump 12 is disposed between the output port 7 and the second flow controller 9, an output end of the air suction pump 12 is further communicated with an exhaust pipe 13, and an exhaust valve 14 is disposed in the exhaust pipe 13.

By arranging the air pump 12, after the gas in the collecting cover 1 is accumulated for a period of time, all the leaked gas in the collecting cover 1 can be pumped into the separating device 2 by the air pump 12 for separation, so that the detection precision is improved.

Simultaneously, make can carry out the preliminary treatment to collecting cover 1 internal environment before detecting the position that awaits measuring, avoid its inside gas to influence the testing result, promptly:

before detection, the air pump 12 and the exhaust valve 14 are opened, and the air pressure in the collecting cover 1 is pumped to negative pressure; the air extracting pump 12 is closed, the gas carrying bottle 4 is opened, the air pressure in the collecting cover 1 is filled to the standard atmospheric pressure, and then the air is continuously filled for 3-5 min; finally, the carrier gas cylinder 4 and the exhaust valve 14 are closed and the test is started. At the moment, the inner space of the collecting cover 1 is inert gas and leakage fluoride gas, so that the influence on the detection result caused by the interference of other gases is avoided.

Wherein, in a preferred embodiment of the separation device 2, the separation device 2 comprises a plurality of detection channels 15 arranged in parallel; one end of the detection channel 15 is communicated with the second flow controller 9, and the other end is communicated with the detection device 3 through a selective valve 16;

each of the detection channels 15 is provided therein with a detection valve 17 and a separation column 18 for separating the leaking gas.

Specifically, the separation device 2 includes a plurality of detection channels 15 arranged in parallel, that is, the number of the detection channels 15 may be one, two or more.

Because the separation device 2 comprises a plurality of detection channels 15 arranged in parallel, and a detection valve 17 and a separation column 18 are arranged in each detection channel 15, the separation cover 1 can be moved to the next measurement position for detection in the process of separating the leaked gas at the detection position.

For example: the separation device 2 comprises two detection channels 15 which are arranged in parallel and are respectively a detection channel and a second detection channel; be equipped with first detection valve and first separation column in the first detection passageway, be equipped with second detection valve and second separation column in the second detection passageway.

When in use, the first detection valve and the second detection valve are closed, and the collection cover 1 is arranged at a first detection position; opening a first detection valve after t time is accumulated; when leakage occurs at the first detection position, the leakage gas can enter the first separation column along the first detection valve for separation;

closing a first detection valve and installing the collection cover 1 at a second detection position while the first separation column performs gas separation; after t time is accumulated, a second detection valve is opened, and when leakage occurs at a second detection position, leaked gas can enter a second separation column along the second detection valve for separation;

through the structure, the first separation column can collect and separate the leaked gas from other positions to be detected while the separation process is carried out, so that the detection time is shortened, and the detection efficiency is improved.

Wherein, in the preferred embodiment of the gas carrier bottle 4, the gas carrier bottle 4 is communicated with the input port 6 through an input pipeline 19; the first flow controller 8 is arranged in the inlet conduit 19; an input valve 20 is arranged in the input pipeline 19 and close to one end of the input port 6.

The input valve 20 is arranged, so that the input pipeline 19 and the collecting cover 1 can be controlled to be switched on and off. Preferably, a first starting valve 23 is arranged on the gas carrying bottle 4, and a second starting valve 24 is arranged on the input device 10.

In the preferred embodiment of the output port 7, the output port 7 is communicated with the separation device 2 through an output pipeline 21, and the second flow controller 9 is arranged in the output pipeline 21.

Wherein, in the preferred embodiment of the collecting port 5, as shown in fig. 2, the collecting port 5 is arranged at the bottom of the collecting cover 1; the collecting cover 1 is provided with a throat hoop 22; a fan 11 is installed in the collecting cover 1.

Specifically, collect cover 1 main part and be the cylinder structure, the collection mouth 5 of its bottom is the arc structure, makes can with the production pipeline lateral wall cooperation is fixed.

Specifically, two ends of the collecting cover 1 are provided with an ear plug 25, the throat hoop 22 is mounted on the ear plug 25, and the throat hoop 22 is used for fixing the collecting cover 1 on the side wall of the production pipeline.

Specifically, collect cover 1 bottom and install sealing washer 27 for it is sealed isolated with external environment to collect cover 1, has improved and has detected the accuracy.

Specifically, through in the collection cover 1 installation fan for can make the gas in the collection cover 1 is comparatively even, the detection of being convenient for.

Example 2

As shown in fig. 3, the present embodiment provides a detection method using the fluoride leak detection apparatus as described above, including the steps of:

s100: and (3) detecting leakage: mounting the collecting hood 1 on a production pipe 26; accumulated t₁Time, the separation device 2 and the detection device 3 are started; when the concentration of the gas output by the detection device 3 is judged to be greater than a set value, the production pipeline 26 has leakage;

specifically, when the gas concentration output by the detection device 3 is determined to be equal to or less than a set value, the production pipe 26 does not have a leak.

Preferably, as shown in fig. 1, since the suction pump 12 is provided between the output port 7 and the second flow controller 9, t is accumulated when the collecting cover 1 accumulates₁After the time, the air pump 12 can be started, so that all the leaked gas in the collecting hood 1 can enter the separating device 2 for separation, and the detection result is more accurate.

Preferably, as shown in fig. 1, the fan 11 may be turned on to make the gas inside the collecting cover 1 more uniform, which is beneficial to improving the detection accuracy.

S200: obtaining a concentration peak area S1 of the fluoride gas: when the concentration peak output by the detection device 3 is judged to be complete, directly obtaining the concentration peak area S1 output by the detection device 3; when the concentration peak shape output by the detection device 3 is judged to be peak clipping, the gas carrying bottle 4 is opened and adjustedThe first flow controller 8 flows Q₁With said second flow controller 9 flow rate Q₂Obtaining a concentration peak area S1 output by the detection device 3;

specifically, Q₁：Q₂99:100 or Q₁：Q₂＝9:10；

S300: injecting standard gas: injecting a volume V into the collecting cover 1 through the input device 10₂Standard gas of (2), cumulative t₂Time, obtaining a concentration peak area S2 output by the detection device 3;

s400: calculating the leakage rate:

wherein q is₁For the concentration of fluoride gas in the leaking gas, q₂Is the fluoride gas concentration in the standard gas.

Specifically, q is₁、q₂Is a known value; wherein q is₁Usually in the range of 100ppb to 100%, q₂Typically 100 ppm;

preferably, the method further comprises the following steps before detecting the leaking gas:

the air pump 12 and the exhaust valve 14 are opened to pump the air pressure in the collecting hood 1 to negative pressure (relative to the standard atmospheric pressure); specifically, the air pressure in the collecting hood 1 was evacuated to 10 kPa.

The air extracting pump 12 is closed, the gas carrying bottle 4 is opened, the air pressure in the collecting cover 1 is filled to the standard atmospheric pressure, and then the air is continuously filled for 3-5 min; the carrier gas cylinder 4 and the exhaust valve 14 are closed.

Preferably, since the separation device 2 comprises a plurality of detection channels 15 arranged in parallel, and a detection valve 17 and a separation column 18 are arranged in each detection channel 15, the separation cover 1 can be moved to the next measurement position for detection during the separation of the leaked gas at the detection position.

Taking the example that the separation device 2 comprises two detection channels 15, that is, the separation device 2 comprises a first detection channel and a second detection channel; meanwhile, a first detection valve and a first separation column are arranged in the first detection channel, and a second detection valve and a second separation column are arranged in the second detection channel; step S100 specifically includes:

mounting the collecting hood 1 at a first inspection position of the production pipe 26, accumulating t₁Time, opening the detection device 3 and the first detection valve; while the first separation column is separated, the collecting hood 1 is mounted at a second detection position of the production pipe 26 and the first detection valve is closed, and t is accumulated₁And (3) opening a second detection valve, enabling the separated gas in the two channels to enter the detection device 3 for detection in sequence through the selective valve 16, and judging that the gas concentration is greater than a set value, and then, leakage exists at the corresponding position.

As can be seen from the above steps, t is accumulated at the position corresponding to the first detection position₁After the time, the leaked gas is separated, and meanwhile, the movable collecting cover 1 is used for detecting the next detection position; the gas separation at each detection position is avoided, and the working efficiency is improved.

It is understood that there may be a plurality of detection channels, and the principle is the same as the above method, which is not described herein again. Preferably, the number of detection channels is less than 10.

The above description is only a preferred embodiment of the application and is illustrative of the principles of the technology employed. It will be appreciated by a person skilled in the art that the scope of the invention as referred to in the present application is not limited to the embodiments with a specific combination of the above-mentioned features, but also covers other embodiments with any combination of the above-mentioned features or their equivalents without departing from the inventive concept. For example, the above features may be replaced with (but not limited to) features having similar functions disclosed in the present application.