CN110940698A - Explosion limit testing device for difficult-to-volatilize liquid and application thereof - Google Patents
Explosion limit testing device for difficult-to-volatilize liquid and application thereof Download PDFInfo
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- CN110940698A CN110940698A CN201811037344.4A CN201811037344A CN110940698A CN 110940698 A CN110940698 A CN 110940698A CN 201811037344 A CN201811037344 A CN 201811037344A CN 110940698 A CN110940698 A CN 110940698A
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- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N25/00—Investigating or analyzing materials by the use of thermal means
- G01N25/50—Investigating or analyzing materials by the use of thermal means by investigating flash-point; by investigating explosibility
- G01N25/54—Investigating or analyzing materials by the use of thermal means by investigating flash-point; by investigating explosibility by determining explosibility
Abstract
The invention relates to an explosion limit testing device for a nonvolatile liquid and application thereof, and mainly solves the problems of inaccurate test result and low automation degree in the prior art. The invention adopts the technical scheme that the explosion limit testing device of the difficult-to-volatilize liquid comprises a digital control system, a temperature control testing system, an ignition observing system and a vacuum air inlet system, wherein the digital control system comprises a numerical control operation screen, a pressure sensor, a thermocouple, an electromagnetic valve and a liquid level sensor, the temperature control testing system comprises a sample chamber, an evaporation chamber, an experimental flask, a temperature control thermocouple, a heating chamber and a heat insulation explosion-proof chamber, the ignition observing system comprises an electric spark igniter, an ignition controller and an observing window, and the vacuum air inlet system comprises a vacuum pump and the application thereof, so that the problems are better solved, and the device can be used for testing the explosion limit of the difficult-to-volatilize liquid.
Description
Technical Field
The invention relates to an explosion limit testing device for a difficult-to-volatilize liquid and application thereof, which are used for testing the explosion limit of the difficult-to-volatilize liquid, viscous liquid and liquid (steam) which can not be injected by a conventional injection method in the air.
Background
Combustible materials (combustible gas, vapor and dust) and air (or oxygen) must be uniformly mixed within a certain concentration range to form premixed gas, and explosion can occur when the premixed gas meets a fire source, wherein the concentration range is called as an explosion limit or an explosion concentration range. For example, the explosion limit of ethanol vapor mixed with air is 3.3% to 19.0%. The lowest and highest concentrations at which a flammable mixture can explode are referred to as the lower explosion limit and the upper explosion limit, respectively, and are sometimes also referred to as the lower and upper fire limits.
The invention relates to a vapor or gas explosion limit test device, which is a set of special devices designed for evaluating the explosion risk of liquid compounds (vapor) in air. The technical requirements of the invention in the aspect of explosion limit test reach the requirements of GB/T21844-2008 standard test method for flammability concentration limit value of compounds (steam or gas) and ASTM E681-04 standard test method for explosion limit of chemicals (steam and gas). At present, the experimental device developed according to the two standards on the market mainly aims at gas or volatile liquid, and problems exist when the hard-to-volatilize liquid is used for mixing and testing, for example, 1. the hard-to-volatilize liquid generally needs higher temperature during testing, the sample cannot be fully preheated by using the existing equipment, the volatilized steam is only a light component, the full component of the sample cannot be fully mixed with air, and the measured lower explosion limit result is increased, so that the explosion limit range is reduced. 2. The existing equipment directly adds a sample into an experimental flask, needs a large amount of sample introduction when measuring a liquid sample which is difficult to volatilize, and can lead the volatilization amount of the incombustible component to be invisibly enlarged when the sample to be measured is a mixture and contains a large amount of incombustible component, thus leading to larger deviation of a test result. 3. The existing device has low automation degree, the sample volume completely depends on the manual control of an operator, so that the existing test method has low efficiency and is easy to generate larger errors.
Disclosure of Invention
The invention aims to solve the technical problems of inaccurate test result and low automation degree in the prior art, provides a novel explosion limit testing device for a nonvolatile liquid, and has the advantages of accurate test result and high automation degree. The second technical problem to be solved by the present invention is to provide a use of the device for testing explosion limit of the nonvolatile liquid corresponding to the first technical problem.
In order to solve one of the problems, the technical scheme adopted by the invention is as follows: the utility model provides an explosion limit testing arrangement of difficult volatile liquid, including digital control system, control by temperature change test system, ignition observation system, vacuum air intake system, digital control system includes the numerical control operation screen, pressure sensor, the thermocouple, the solenoid valve, the liquid level inductor, control by temperature change test system includes the sampling room, the evaporating chamber, the laboratory flask, accuse temperature thermocouple, the heating chamber, thermal-insulated explosion-proof room, ignition observation system includes spark ignition ware, ignition controller, the observation window, vacuum air intake system includes the air intake pipe, the vacuum pump, the gas circuit connecting pipe, the sampling room links to each other with the evaporating chamber, the laboratory flask is located thermal-insulated explosion-proof room, be equipped with spark ignition ware in the laboratory flask.
In the above technical solution, preferably, the sampling chamber, the evaporation chamber, the laboratory flask, and the vacuum pump are connected through a connection sleeve, and the connection degree is controlled by an electromagnetic valve.
In the above technical solution, preferably, the experimental flask is placed in the middle of the upper half part of the heat-insulating explosion-proof chamber, and the evaporation chamber is placed on the left side of the lower half part of the heat-insulating explosion-proof chamber.
In the above technical scheme, preferably, the bottom protrusions of the evaporation chamber and the heat-insulating explosion-proof chamber are provided with stirrers.
In the above technical scheme, preferably, a liquid level sensor is arranged in the evaporation chamber.
In the above technical solution, preferably, a solenoid valve is disposed on a pipeline connecting the sampling chamber and the evaporation chamber.
In the above technical scheme, preferably, the bottom of the heat-insulating explosion-proof chamber is provided with a pipeline connected with the evaporation chamber, and the connected pipeline is provided with an electromagnetic valve.
In the above technical solution, preferably, the connection between the digital control system and the ignition observation system is realized by each thermocouple, electromagnetic valve, and pressure sensor, which are directly connected to the processor of the numerical control operation screen, and the temperature and pressure changes of each part in the system are measured on line, and the relevant data is fed back in time, and the on-off of each electromagnetic valve is controlled according to a preset program.
In the above technical solution, preferably, during the test, the vacuum pump is turned on to evacuate the evaporation chamber and the experimental flask, then the sample in the sample chamber is introduced into the evaporation chamber, and the vapor generated by the sample is introduced into the experimental flask after the sample is fully preheated.
In order to solve the second problem, the invention adopts the following technical scheme: the explosion limit testing device of the nonvolatile liquid is applied to the explosion limit testing of the nonvolatile liquid.
This patent is one set and is used for surveing difficult volatile liquid and glues the explosion limit testing arrangement who is difficult to the liquid of injecting the appearance, and testing arrangement in the past can obtain more accurate result only generally when the explosion limit of test gas and volatile liquid, and is inaccurate when measuring the explosion limit of non-volatile liquid, and the collection of advance appearance and data simultaneously all does not realize the automation. Three advantages of the explosion limit test are achieved compared to conventional devices: (1) the test sample is fully preheated, and the sample steam directly reaches the experimental flask from the steam chamber, so that the intermediate link is shortened, the heat loss of the sample steam is reduced, and the test result is more in line with the actual value under the set reaction condition. (2) The volatilization conditions of the liquid chemicals which are not easy to volatilize in the actual production, storage and transportation processes are better simulated, and the error generated when the mixed gas of the sample steam and the air is prepared by the existing testing instrument in the actual application process is reduced. (3) Through increasing digital control system, set up corresponding kind concentration of advancing, use the electromagnetic valve control sample steam advance kind and prepare and mix the gas, reduced by the error that operating personnel manual operation advances kind and produces, improved efficiency of software testing, gained better technological effect.
Drawings
FIG. 1 is a schematic flow diagram of the apparatus of the present invention.
In fig. 1: A. a fastening cover clip with a spring; B. a heat-insulating explosion-proof chamber; C. a heating device; D. a thermocouple; E. a sample introduction chamber; F. emergency discharge; G. a liquid level sensor; H. a liquid discharge port; I. a numerical control operation screen; J. an observation window; K. an electric spark ignition electrode; l, a stirring device; m, a vacuum pump; n, stabilizing the support; o. evaporation chamber.
The present invention will be further illustrated by the following examples, but is not limited to these examples.
Detailed Description
[ example 1 ]
An explosion limit testing device for a nonvolatile liquid is shown in figure 1 and comprises a digital control system, a temperature control testing system, an ignition observation system and a vacuum air inlet system.
1. The system comprises the following components:
the digital control system comprises: numerical control operation screen, pressure sensor, thermocouple, solenoid valve, liquid level sensor etc..
Temperature control test system: a sample chamber, an evaporation chamber, a laboratory flask, a temperature control thermocouple, a heating chamber, a heat insulation explosion-proof chamber and the like.
Ignition observation system: an electric spark igniter, an ignition controller, an observation window, etc.
A vacuum air inlet system: an air inlet pipe, a vacuum pump, an air path connecting pipe and the like.
2. The connection relation of each component is as follows:
the sampling chamber, the evaporation chamber, the experimental flask and the vacuum pump are connected through a connecting sleeve, and the connection degree is controlled by an electromagnetic valve. The experimental flask was placed in the middle of the upper half of the insulated explosion-proof chamber. The evaporation chamber is arranged on the left side of the lower half part of the heat-insulating explosion-proof chamber. And two stirrers are positioned in the evaporation chamber, and one stirrer is positioned at the bulge at the bottom of the heat-insulating explosion-proof chamber.
In the test, the vacuum pump is firstly turned on to vacuumize the evaporation chamber and the experimental flask, then the sample in the sampling chamber is introduced into the evaporation chamber, and the vapor generated by the sample is introduced into the experimental flask after the sample is fully preheated.
The digital control system is connected with the ignition observation system through each thermocouple, electromagnetic valve, pressure sensor and the like, which are directly connected with a processor of the numerical control operation screen, and the temperature and pressure changes of each part in the system are measured on line, the relevant data are fed back in time, and the on-off of each electromagnetic valve is controlled according to a preset program.
When the device is used, the test needs to be carried out in a fume hood, an exhaust system is suitable for absorbing toxic smoke, an experimenter needs to wear an explosion-proof helmet, goggles and protective gloves before operation, and then the test is carried out according to the following steps:
1. the device is connected as shown in fig. 1, the numerical control operation screen is opened, and the experiment temperature and the sample injection amount are preset. The electromagnetic valves 2 and 3 are automatically opened, the vacuum pump is started to vacuumize, and the process is repeated for at least 3 times.
2. And after the vacuumizing is finished, adding at least 250ml of liquid sample into the sample chamber, closing the electromagnetic valves 2 and 3 and the vacuum pump, opening the electromagnetic valve 1 to enable the sample to flow into the evaporation chamber, and closing the electromagnetic valve 1 when the liquid level detector detects that the liquid amount in the evaporation chamber reaches 200 ml. The heating device and the stirrer start.
3. When the temperature in the evaporation chamber and the laboratory flask reached the set value and stabilized for at least 5min, the solenoid valve 2 was opened and the sample vapor started to enter the laboratory flask.
4. When the concentration of the sample reaches a set value (judged by calculating the partial pressure of the sample vapor), the electromagnetic valve 2 is closed, the electromagnetic valves 3 and 4 are opened, and the introduction of the sample vapor is stopped and the introduction of air is started.
5. When the pressure in the experimental flask reached substantially the same pressure as real-time atmospheric pressure, solenoid valves 3, 4 were closed. Waiting at least 5min allowed the air and sample vapors to be well mixed and heated in the experimental flask.
6. And (3) closing the stirrer, checking whether the heat-insulating explosion-proof chamber is completely closed, taking down the ignition controller, stretching the connecting wire as far as possible, and simultaneously pressing two buttons on the ignition controller to ignite.
7. And observing whether flame propagates or not through the observation window.
According to the analysis requirements of GB/T21844-.
[ example 2 ]
The apparatus was used in the absolute ethanol explosion limit test according to the conditions and procedures described in example 1.
1. The apparatus was connected as shown in fig. 1, the numerically controlled operation panel was opened, the test temperature was set to 50 ℃ and the sample concentration was set to 3 kPa. The electromagnetic valves 2 and 3 are automatically opened, the vacuum pump is started to vacuumize, and the process is repeated for at least 3 times.
2. After the vacuum pumping is finished, at least 250ml of ethanol sample is added into the sample chamber, the electromagnetic valves 2 and 3 and the vacuum pump are closed, the electromagnetic valve 1 is opened to enable the ethanol sample to flow into the evaporation chamber, and when the liquid level detector detects that the liquid amount in the evaporation chamber reaches 200ml, the electromagnetic valve 1 is closed. The heating device and the stirrer start.
3. When the temperature in the evaporation chamber and the laboratory flask reached 30 ℃ and stabilized for at least 5min, solenoid valve 2 was opened and sample vapor began to enter the laboratory flask.
4. When the concentration of the sample reaches a set value (judged by calculating the partial pressure of the sample vapor), the electromagnetic valve 2 is closed, the electromagnetic valves 3 and 4 are opened, and the introduction of the sample vapor is stopped and the introduction of air is started.
5. When the pressure in the experimental flask reached substantially the same pressure as real-time atmospheric pressure, solenoid valves 3, 4 were closed. Wait for at least
5min allowed air and sample vapors to be thoroughly mixed and heated in the experimental flask.
6. And (3) closing the stirrer, checking whether the heat-insulating explosion-proof chamber is completely closed, taking down the ignition controller, stretching the connecting wire as far as possible, and simultaneously pressing two buttons on the ignition controller to ignite.
7. And observing whether flame propagates or not through the observation window.
According to the analysis requirements of GB/T21844-.
TABLE 1
The requirement for precision and error according to GB/T21844-: the lower limit of combustion is not more than 0.9%, the upper limit of combustion is not more than 1.8% ", and the error of the test result meets the requirement.
[ example 3 ]
The apparatus was used in the acrylic varnish explosion limit test according to the conditions and procedures described in example 1.
1. The apparatus was connected as shown in fig. 1, the numerically controlled operation panel was opened, the test temperature was set to 100 ℃ and the sample concentration was set to 1 kPa. The electromagnetic valves 2 and 3 are automatically opened, the vacuum pump is started to vacuumize, and the process is repeated for at least 3 times.
2. And after the vacuumizing is finished, adding at least 250ml of acrylic acid varnish sample into the sample chamber, closing the electromagnetic valves 2 and 3 and the vacuum pump, opening the electromagnetic valve 1 to enable the acrylic acid varnish sample to flow into the evaporation chamber, and closing the electromagnetic valve 1 when the liquid level detector detects that the liquid amount in the evaporation chamber reaches 200 ml. The heating device and the stirrer start.
3. When the temperature in the evaporation chamber and the laboratory flask reached 30 ℃ and stabilized for at least 5min, solenoid valve 2 was opened and sample vapor began to enter the laboratory flask.
4. When the concentration of the sample reaches a set value (judged by calculating the partial pressure of the sample vapor), the electromagnetic valve 2 is closed, the electromagnetic valves 3 and 4 are opened, and the introduction of the sample vapor is stopped and the introduction of air is started.
5. When the pressure in the experimental flask reached substantially the same pressure as real-time atmospheric pressure, solenoid valves 3, 4 were closed. Waiting at least 5min allowed the air and sample vapors to be well mixed and heated in the experimental flask.
6. And (3) closing the stirrer, checking whether the heat-insulating explosion-proof chamber is completely closed, taking down the ignition controller, stretching the connecting wire as far as possible, and simultaneously pressing two buttons on the ignition controller to ignite.
7. And observing whether flame propagates or not through the observation window.
According to the analysis requirements of GB/T21844-. Due to the complex composition of the sample and lack of literature values, the comparison was performed by repeating the test 10 times, as shown in table 2.
TABLE 2
| Number of tests | Lower explosion limit (%) | Upper explosion limit (%) |
| 1 | 3.9 | 8.1 |
| 2 | 3.8 | 7.9 |
| 3 | 4.0 | 8.2 |
| 4 | 3.9 | 7.9 |
| 5 | 4.0 | 7.8 |
| 6 | 3.8 | 8.0 |
| 7 | 3.9 | 7.9 |
| 8 | 4.0 | 8.2 |
| 9 | 4.0 | 7.8 |
| 10 | 3.9 | 8.1 |
| Maximum repeatability error | 0.2 | 0.4 |
According to the requirements of precision and error of GB/T21844-: the lower limit of combustion is not more than 0.2%, the upper limit of combustion is not more than 0.8% ", and the error of the test result meets the requirement.
Claims (10)
1. The utility model provides an explosion limit testing arrangement of difficult volatile liquid, including digital control system, control by temperature change test system, ignition observation system, vacuum air intake system, digital control system includes the numerical control operation screen, pressure sensor, the thermocouple, the solenoid valve, the liquid level inductor, control by temperature change test system includes the sampling room, the evaporating chamber, the laboratory flask, accuse temperature thermocouple, the heating chamber, thermal-insulated explosion-proof room, ignition observation system includes spark ignition ware, ignition controller, the observation window, vacuum air intake system includes the air intake pipe, the vacuum pump, the gas circuit connecting pipe, the sampling room links to each other with the evaporating chamber, the laboratory flask is located thermal-insulated explosion-proof room, be equipped with spark ignition ware in the laboratory flask.
2. The apparatus for testing explosion limit of a nonvolatile liquid as claimed in claim 1, wherein the sample chamber, the evaporation chamber, the laboratory flask, and the vacuum pump are connected via a connecting sleeve, and the connection degree is controlled by an electromagnetic valve.
3. The explosion limit testing device of a nonvolatile liquid as in claim 1, wherein the test flask is placed in the middle of the upper half of the thermal insulation explosion-proof chamber, and the evaporation chamber is placed on the left side of the lower half of the thermal insulation explosion-proof chamber.
4. The explosion limit testing device of the nonvolatile liquid as claimed in claim 1, wherein stirrers are provided at the bottom protrusions of the evaporation chamber and the thermal insulation explosion-proof chamber.
5. The explosion limit testing device of a nonvolatile liquid as claimed in claim 1, wherein a liquid level sensor is provided in the evaporation chamber.
6. The apparatus for testing explosion limit of a nonvolatile liquid as claimed in claim 1, wherein a solenoid valve is provided on a line connecting the sample introduction chamber and the evaporation chamber.
7. The explosion limit testing device of a nonvolatile liquid as claimed in claim 1, wherein the bottom of the heat-insulating explosion-proof chamber is provided with a pipeline connected with the evaporation chamber, and the pipeline connected with the evaporation chamber is provided with an electromagnetic valve.
8. The explosion limit testing device of the nonvolatile liquid as claimed in claim 1, wherein the connection between the digital control system and the ignition observing system is realized by each thermocouple, electromagnetic valve, and pressure sensor, which are directly connected with the processor of the numerical control operation panel, and the temperature and pressure changes of each part in the online measuring system are fed back to the relevant data in time, and the on-off of each electromagnetic valve is controlled according to a preset program.
9. The apparatus for testing explosion limit of a nonvolatile liquid as claimed in claim 1, wherein, in the test, the vacuum pump is firstly turned on to evacuate the evaporation chamber and the test flask, then the sample in the sample chamber is introduced into the evaporation chamber, and the vapor generated by the sample is introduced into the test flask after the sample is fully preheated.
10. Use of the device for testing the explosive limit of a nonvolatile liquid according to claims 1 to 9 for testing the explosive limit of a nonvolatile liquid.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111380911A (en) * | 2020-05-07 | 2020-07-07 | 中北大学 | Device and method for testing critical explosion temperature of explosive substance solution |
| CN111380909A (en) * | 2020-05-07 | 2020-07-07 | 中北大学 | Critical explosion temperature testing container for explosive material solution |
| CN111380910A (en) * | 2020-05-07 | 2020-07-07 | 中北大学 | Device for testing critical explosion temperature of explosive substance solution |
| CN111879819A (en) * | 2020-07-31 | 2020-11-03 | 上海化工研究院有限公司 | Closed-loop circulating type volatile liquid explosion limit measuring device |
| CN113075258A (en) * | 2020-01-03 | 2021-07-06 | 应急管理部化学品登记中心 | Explosion limit testing device for difficult-to-volatilize liquid and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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