Disclosure of Invention
In view of the above, the invention provides a synchronous test analysis device and method for oxygen consumption and products of a mine reactive polymer material smoldering process, aiming at solving the problems that the existing smoldering process test device is only limited to test the temperature evolution characteristics of different positions in the mine reactive polymer material smoldering process, and synchronous analysis and test of oxygen consumption, smoke generation and toxic and harmful gases in the smoldering process cannot be realized.
In order to achieve the aim, the invention provides a synchronous experimental analysis device for smoldering oxygen consumption and products of mine high polymer materials, which comprises a test gas storage tank, a smoldering reaction chamber for placing mine reaction type high polymer material solidified bodies and a smoldering product collecting tank connected to the gas outlet side of the smoldering reaction chamber, wherein an oxygen bottle with a pressure reducing valve I and a nitrogen bottle with a pressure reducing valve II are connected to the test gas storage tank through pipelines, an oxygen concentration sensor I is also installed on the test gas storage tank, a heating device which is controlled by a computer and is used for heating the mine reaction type high polymer material solidified bodies and a thermocouple which is convenient for testing the temperature change of different positions of the mine reaction type high polymer material solidified bodies are arranged in the smoldering reaction chamber, the test gas storage tank is communicated with the mine reaction type high polymer material solidified bodies through a pipeline with a gas pressure measuring device and a gas flow control device, and a pore plate flowmeter with a gas flow indicator and an oxygen concentration sensor II are arranged on a connecting pipeline between the smoldering product collecting tank and the smoldering reaction chamber, and a smoke sampling device, a mass flow meter and an air bag are also arranged on a pipeline between the smoldering product collecting tank and the oxygen concentration sensor II.
Further, the outside of the mine reactive polymer material curing body is coated with a honeycomb ceramic ring, an exhaust pump with a needle valve is installed on the smoldering reaction chamber, a vacuum thermocouple meter is installed on the test gas storage tank, a draw-out fan is installed on a pipeline on the left side of the oxygen concentration sensor II, and a gas pressurizing device is installed on a pipeline on the right side of the oxygen concentration sensor II.
A synchronous experimental analysis method for smoldering oxygen consumption and product of a mining high polymer material comprises the following steps:
s1: closing a needle valve I on an oxygen cylinder, a needle valve II on a nitrogen cylinder and a needle valve III on an exhaust pipeline of a smoldering reaction chamber, opening a needle valve IV on a connecting pipeline of a test gas storage tank and the smoldering reaction chamber, simultaneously opening an exhaust pump to carry out vacuum degassing on the test gas storage tank and an air inlet pipeline for gas distribution, and closing the needle valve IV and the exhaust pump until the index of a vacuum thermocouple meter arranged on the test gas storage tank is less than or equal to 20;
s2: opening a needle valve I and a needle valve II, opening a pressure reducing valve I on an oxygen cylinder and a pressure reducing valve II on a nitrogen cylinder, and configuring test gas in a test gas storage tank to enable the numerical value of an oxygen concentration sensor I to meet the experimental requirements; if the readings of the oxygen concentration sensor I on the test gas storage tank are the values required by the test, closing the needle valve I, the needle valve II, the pressure reducing valve I and the pressure reducing valve II; if the index of an oxygen concentration sensor I on the test gas storage tank does not reach the numerical value required by the test, closing a needle valve I, a needle valve II, a pressure reducing valve I and a pressure reducing valve II, opening a needle valve IV, starting an exhaust pump to exhaust the test gas storage tank, then closing the needle valve IV and the exhaust pump, opening the needle valve I, the needle valve II, the pressure reducing valve I and the pressure reducing valve II again, and configuring the test gas for the test gas storage tank until the numerical value of the oxygen concentration sensor I meets the experimental requirement;
s3: placing the mine reaction type high polymer material solidified body formed after solidification in a honeycomb ceramic ring, and then placing the honeycomb ceramic ring in a smoldering reaction chamber; opening a needle valve III, closing a needle valve V between a smoldering product collecting tank and a smoldering reaction chamber and a needle valve VI between a smoke sampling device and an air bag, and opening an exhaust pump to exhaust the smoldering reaction chamber, an air outlet pipeline of the smoldering reaction chamber and the smoldering product collecting tank; then opening the needle valve V and the needle valve VI, and opening the needle valve III; adjusting a pressure reducing valve III between the test gas storage tank and the smoldering reaction chamber to enable the test gas in the test gas storage tank to flow out, and monitoring the pressure of the test gas through a gas pressure measuring device to enable the value of the pressure to be higher than 0.1 MPa; and simultaneously adjusting the gas flow control device to enable the flow of the test gas to reach the numerical value required by the test;
s4: starting a heating device to heat the mine reaction type high polymer material solidified body, and adjusting the heating rate according to the test requirement; meanwhile, starting a thermocouple, a gas flow indicator, an oxygen concentration sensor II, a gas pressurizing device and a draw-out fan;
s5: in the test process, sampling the smoke in the pipeline through a smoke sampling device arranged on the pipeline at intervals according to the test requirements; opening the needle valve VI and the mass flowmeter while sampling the smoke, enabling part of gas after smoldering reaction to enter the air bag, simultaneously recording the readings of a gas flow indicator connected with the orifice plate flowmeter and the readings of an oxygen concentration sensor II, and controlling the sampling time within 60 s;
s6: when the reading of the oxygen concentration sensor II is equal to that of the oxygen concentration sensor I and the reading of a gas flow indicator arranged on the orifice plate flowmeter is equal to the flow controlled by the gas flow control device, indicating that smoldering reaction is finished, immediately closing the heating device, the pressure reducing valve III, the gas flow control device, the gas flow indicator, the extraction type fan, the gas pressurizing device, the needle valve V and the mass flowmeter;
s7: weighing the smoke sample obtained each time, and obtaining the obtained smoke mass, which is recorded as myt(ii) a Obtaining the smoke yield within the corresponding sampling time 60 s; obtaining the smoke generation rate at the corresponding moment in the test process, drawing a curve of the smoke generation rate changing along with time, obtaining a polynomial expression of the curve of the smoke generation rate changing along with time by adopting a polynomial fitting method, and then obtaining the accumulated smoke yield in the test process by adopting an integration method;
s8: multiplying the readings of the oxygen concentration sensor I and the oxygen concentration sensor II in each sampling by the readings of the gas flow control device and the readings of the gas flow indicator arranged on the orifice plate flowmeter respectively, and obtaining the smoldering oxygen consumption speed of the mine reaction type high polymer material solidified body corresponding to each sampling through data processing; then drawing a curve of smoldering oxygen consumption speed of the mine reaction type high polymer material solidified body changing along with time, obtaining a polynomial expression of the curve of smoldering oxygen consumption speed of the mine reaction type high polymer material solidified body changing along with time by adopting a polynomial fitting method, and obtaining accumulated oxygen consumption in the test process by adopting an integral method;
s9: performing component analysis on the gas collected in the air bag each time by using a gas chromatography analysis method to obtain the concentration of corresponding combustible or harmful gas; and multiplying the numerical value by the index of the mass flow meter to obtain the output rate of the combustible or harmful gas within the corresponding sampling time of 60s, drawing a curve of the output rate and the speed of the combustible or harmful gas changing along with time, obtaining a polynomial expression of the curve of the output rate of the combustible or harmful gas changing along with time by adopting a polynomial fitting method, and obtaining the quantity of the combustible or harmful gas in the test process by adopting an integration method.
Further, step S2 specifically includes the following steps:
s21: according to the oxygen concentration of the mine reactive polymer material in the underground coal mine application environment, test gas is configured for the test gas storage tank, so that the value of an oxygen concentration sensor I of the test gas storage tank meets the experimental requirements, and the configured oxygen concentration needs to be consistent with the value of the oxygen concentration of the mine reactive polymer material in the underground coal mine application environment;
s22: when the test gas is configured, attention should be paid to observing the readings of the oxygen concentration sensor I on the test gas storage tank, and if the values meet the test requirements, the configuration of the test gas is stopped;
s23: when the test gas is configured, if the index of the oxygen concentration sensor I on the test gas storage tank is lower than the numerical value required by the test, the pressure reducing valve II and the needle valve II on the high-pressure nitrogen cylinder are closed, the pressure reducing valve I and the needle valve I on the high-pressure oxygen cylinder are continuously kept open, the high-pressure oxygen is continuously injected into the test gas storage tank, and the index C of the oxygen concentration sensor I on the to-be-tested gas storage tank1After the test requirements are met, stopping configuring the test gas;
s24: when the test gas is supplied, if the indication C of the oxygen concentration sensor I on the test gas storage tank1If the value is higher than the test requirement, closing the pressure reducing valve II and the needle valve II on the high-pressure nitrogen cylinder and the pressure reducing valve I and the needle valve I on the high-pressure oxygen cylinder, and opening the exhaust pump to store the test gasAnd (3) exhausting gas in the collecting tank, then closing the needle valve IV and the exhaust pump, opening the needle valve I, the needle valve II, the pressure reducing valve I on the oxygen cylinder and the pressure reducing valve II on the nitrogen cylinder again, and configuring the test gas in the test gas storage tank until the numerical value of the oxygen concentration sensor meets the requirements of the experiment.
Further, step S3 specifically includes the following steps:
s31: the mine reaction type high polymer material solidified body is formed by pouring two chemical solutions into a specific mould according to the actual application requirements of the underground coal mine, wherein the mould is a plastic drum with the same inner diameter and height as the honeycomb ceramic ring; the honeycomb ceramic ring wall is hollow, and openings are formed in the inner wall and the outer wall, so that a flowing channel is provided for test gas, and the test gas is in contact with the outer surface of the mining reaction type high polymer material curing body; after the mine reactive polymer material is fully reacted, immediately forming a corresponding solidified body, then removing the die by using a blade, and placing the mine reactive polymer material solidified body in the honeycomb ceramic ring; then placing the honeycomb ceramic ring with the mine reaction type high polymer material solidified body into a smoldering reaction chamber;
s32: the smoldering reaction chamber has an outer wall made of stainless steel and an inner wall made of nano microporous material, and has the functions of providing space for the smoldering chemical reaction of the mine reactive high polymer material and preventing the smoldering process from being influenced by the external temperature; one end of the smoldering reaction chamber is provided with a flange which is matched with a flange on the heating device to realize connection; the flange is provided with bolt holes, and the flange is fastened by bolts during connection; the end faces of the flanges are provided with circular grooves, and high-temperature-resistant rubber rings are placed in the circular grooves when the flanges are connected, so that the end faces of the two flanges are sealed, the gas in a smoldering reaction chamber is prevented from leaking, and the reliability of a test result is ensured; the heating device is used for heating the mine reaction type high polymer material solidified body, and the starting and heating rates of the heating device are controlled by a computer connected with the heating device;
s33: opening the needle valve III, closing the needle valve V and the needle valve VI, and opening an exhaust pump to exhaust the smoldering reaction chamber, the gas outlet pipeline of the smoldering reaction chamber and the smoldering product collecting tank so as to eliminate the influence of external air entering the smoldering reaction chamber, the gas outlet pipeline of the smoldering reaction chamber and the smoldering product collecting tank on the test result in the assembling process of the test device and the mine reaction type high polymer material solidified body test piece; the inner walls of the gas outlet pipeline of the smoldering reaction chamber and the smoldering product collecting tank are both sprayed with nano materials, and the function of the nano materials is to ensure that smoke generated in the test process is not adsorbed on the inner walls of the gas outlet pipeline of the smoldering reaction chamber and the smoldering product collecting tank;
s34: the pressure reducing valve III on the test gas storage tank enables the test gas in the test gas storage tank to flow out, the pressure of the test gas is monitored through a gas pressure measuring device, the numerical value of the pressure is 0.1-0.11 MPa, the test gas in the test gas storage tank flows out through adjusting the pressure reducing valve III, and the pressure of the flowing test gas is monitored through the gas pressure measuring device; the space atmospheric pressure applied by the mine underground reactive high polymer material is 0.1MPa, and when a draw-out fan arranged on the gas outlet side of the smoldering reaction chamber operates, a certain pressure difference is generated to enable the test gas to flow in the smoldering reaction chamber and a pipeline, so that the pressure of the flowing-out test gas is required to be 0.1-0.11 MPa, and the pressure of the test gas contacting with the mine reactive high polymer material test piece in the smoldering reaction chamber is close to the underground atmospheric pressure of the coal mine;
s35: simultaneously adjusting the gas flow control device to make the flow of the test gas reach the value required by the test, and defining the value as VjThe value V ofjThe method is characterized in that the flow of the test gas flowing out of the test gas storage tank is adjusted according to the flow velocity of the wind flow in the working condition environment of the mine reactive polymer material used underground in the coal mine, so that the flow velocity of the test gas contacted with the test piece of the mine reactive polymer material solidified body in the smoldering reaction chamber is close to the wind flow velocity in the actual working condition environment.
Further, step S4 specifically includes the following steps:
s41: the heating device is controlled by a computer, and the heating rate of the heating device is adjusted and controlled by the computer to meet the requirements of a test scheme;
s42: the thermocouple is inserted into the interior of the mine reaction type high polymer material solidified body and is used for measuring the change of the internal temperature field of the mine reaction type high polymer material solidified body in the smoldering test process, the measured temperature data is transmitted to the computer, and the temperature change of different positions in the mine reaction type high polymer material solidified body at different time in the whole smoldering test process is obtained through data processing;
s43: the gas flow indicator is connected to the gas inlet side and the gas outlet side of the orifice plate flowmeter through a pressure measuring pipeline, and the flow Vc of the test gas after passing through the mine reactive polymer material solidified body is obtained by calculating the gas pressure difference between the two ends of the gas inlet side and the gas outlet side of the orifice plate flowmeter; the straight pipe section on the air inlet side of the orifice plate flowmeter is more than or equal to 10 times of the inner diameter of the pipeline, and the straight pipe section on the air outlet side of the orifice plate flowmeter is more than or equal to 5 times of the inner diameter of the pipeline; the oxygen concentration sensor II is used for monitoring the oxygen concentration value C of the test gas in the pipeline after the test gas passes through the mine reaction type high polymer material solidified body2;
S44: the gas pressurizing device is used for pressurizing and conveying the gas passing through the mine reaction type high polymer material solidified body into the smoldering product collecting tank, and the volume of the smoldering product collecting tank is Vs;
S45: the surfaces of the blades and the flow channel of the draw-out fan are sprayed with nano materials, and the effect of the nano materials is to prevent smoke generated in the smoldering test process from being attached to the surfaces of the blades and the flow channel of the draw-out fan, so that the influence on the final calculation of the smoke yield in the whole smoldering process is caused.
Further, step S5 specifically includes the following steps:
s51: the smoke sampling device is connected with an air outlet pipeline of the smoldering reaction chamber through a flange; the sampling device consists of a short-circuit pipeline and an upper sampling device; the inner diameter and the outer diameter of the short-circuit pipeline are the same as those of the gas outlet pipeline of the smoldering reaction chamber; the quarter circular arc part of the short-circuit pipeline is connected with the pipeline through a hinge structure, the quarter circular arc part of the short-circuit pipeline is connected with a push rod II in the sampling device at the upper part through an iron wire, the push rod II is of a piston structure, and when the push rod II is pulled outwards, the quarter circular arc part of the short-circuit pipeline is separated from the short-circuit pipeline; the part of the short-circuit pipeline, the top of which is contacted with the quarter-arc part, adopts the magnet, and when sampling is not needed, the magnet attracts the quarter-arc part to prevent gas in the pipeline from leaking; when sampling, pulling the push rod II to separate the quarter arc part of the short-circuit pipeline from the short-circuit pipeline, and then pushing the push rod I downwards to drive the filter membrane bracket to move to the quarter arc part of the original short-circuit pipeline; the filter membrane bracket is made of plastic, and the outer surface of the filter membrane bracket is sprayed with nano materials to prevent smoke from attaching to the filter membrane bracket; a filter membrane is further arranged on the filter membrane bracket, and the area of the filter membrane is equal to one fourth of the area of the inner section of the pipeline;
s52: when sampling, recording the time t for starting samplingqAfter 60s, pulling the push rod I to take out the filter membrane, and then pushing the push rod II to connect the quarter circular arc part of the short-circuit pipeline with the short-circuit pipeline;
s53: opening the needle valve VI and the mass flowmeter during sampling to ensure that part of gas after smoldering reaction enters the air bag, and recording the accumulated flow in the sampling period of 60s as Vqt(ii) a And simultaneously recording the indication Vc of a gas flow indicator connected with the orifice plate flowmeter and the indication C of an oxygen concentration sensor II2t。
8. The mining polymer material smoldering oxygen consumption and product synchronous test analysis method of claim 3, characterized in that step S7 specifically comprises the following steps:
s71: the mass of the filter membrane before and after sampling was weighed to obtain a mass of 4m of the smoke generated within 60s of the samplingytThe generating speed of the smoke is 4m in the smoldering process of the mine reaction type high polymer material solidified bodyyt/min;
S72: then the generation rates m of the smoke at different sampling times obtained in the whole test process are comparedytAnd/min, drawing a corresponding curve changing along with time, obtaining a polynomial expression of the curve changing along with time of the smoke generation rate by adopting a polynomial fitting method, and marking as: f (m)yt);
S73: the obtained polynomial expression f (m)
yt) Determining the duration t of the entire smoldering test procedure
zThe integration of (1):
i.e. the cumulative smoke yield during the test.
Further, step S8 specifically includes the following steps:
s81: will (V)j×C1-Vc×C2) Calculating to obtain the smoldering oxygen consumption speed h of the mine reaction type high polymer material solidified body in each samplingtDimension of m3Min; then drawing a curve of smoldering oxygen consumption speed of the mine reaction type high polymer material solidified body changing along with time, and obtaining a polynomial expression lambda (h) of the curve of smoldering oxygen consumption speed of the mine reaction type high polymer material solidified body changing along with time by adopting a polynomial fitting methodt);
S82: the polynomial expression λ (h) to be obtained
t) Determining the duration t of the entire smoldering test procedure
zThe integration of (1):
namely the accumulated smoldering oxygen consumption of the mine reaction type high polymer material solidified body in the test process.
Further, step S9 specifically includes the following steps:
s91: connecting the air bag with a gas chromatography device, and analyzing to obtain the concentration of corresponding combustible or harmful gas CqtAnd multiplying the value by the reading M of the mass flow meterqtNamely: (C)qt×Mqt) The output rate of combustible or harmful gas within 60s of corresponding sampling time is (C)qt×Mqt)/min;
S92: then the generation rate of combustible or harmful gas at different sampling time obtained in the whole test process is (C)qt×Mqt) And/min, drawing a corresponding curve changing along with time, obtaining a polynomial expression of the curve changing along with the time t of the generation rate of the combustible or harmful gas by adopting a polynomial fitting method, and marking as: ψ (t);
s93: the obtained polynomial expression psi (t) is solved to obtain the whole smoldering combustion experimentDuration t of the program
zThe integration of (1):
i.e. the cumulative amount of combustible or hazardous gas produced during the test.
The invention has the beneficial effects that:
the invention provides a synchronous test analysis method and a synchronous test analysis device for oxygen consumption and products of a mine reaction type high polymer material smoldering overall process, which can accurately realize synchronous determination of the oxygen consumption and the products of the mine reaction type high polymer material smoldering overall process, and compared with the prior experiment method, the synchronous test analysis method and the synchronous test analysis device for the oxygen consumption and the products of the mine reaction type high polymer material smoldering overall process have the following advantages:
1. the synchronous test analysis method for the total oxygen consumption and the product of the mine reactive polymer material smoldering process can realize accurate preparation of test gas, truly reduce the oxygen atmosphere in the application environment of the mine reactive polymer material under the coal mine, and adjust the oxygen concentration in the test gas according to the oxygen concentration values in different application environments under the coal mine.
2. The synchronous test analysis method for the total oxygen consumption and the product of the mine reactive polymer material smoldering process can accurately control the flow of the test gas contacting with the mine reactive polymer material solidified body, further simulate the influence of the smoldering process of the mine reactive polymer material solidified body under the condition of gas flow velocity in different underground coal mine application environments, and provide technical support for objectively evaluating the application safety performance of the mine reactive polymer material.
3. The synchronous test analysis method for the oxygen consumption and the product in the whole smoldering process of the mine reactive high polymer material can collect smoke, combustible or harmful gas at any time in the smoldering test process, and can accurately calculate the corresponding output rate; furthermore, corresponding polynomial functions are obtained by fitting the change of the output rate of the smoke, the combustible or the harmful gas along with the smoldering time, and the accumulated amount of the smoke, the combustible or the harmful gas in the smoldering test process is finally obtained by adopting an integration method, so that a solid foundation is laid for researching the mapping rule of the smoldering products and the time of the mine reactive high polymer material.
4. According to the synchronous test analysis method for the oxygen consumption and the product in the whole smoldering process of the mine reactive polymer material, provided by the invention, the oxygen consumption of the mine reactive polymer material under different time conditions in the smoldering test process can be calculated through the oxygen concentration and the gas flow of the gas inlet end and the gas outlet end of a smoldering reaction chamber, so that a technical support is provided for researching the oxygen consumption rule of the mine reactive polymer material in the smoldering process.
Additional advantages, objects, and features of the invention will be set forth in part in the description which follows and in part will become apparent to those having ordinary skill in the art upon examination of the following or may be learned from practice of the invention. The objectives and other advantages of the invention will be realized and attained by the structure particularly pointed out in the written description and claims hereof as well as the appended drawings.
Detailed Description
Preferred embodiments of the present invention will be described in detail below with reference to the accompanying drawings.
Reference numerals in the drawings of the specification include:
the device comprises a needle valve I1, a needle valve II 2, a needle valve III 3, a needle valve IV 4, an exhaust pump 5, a test gas storage tank 6, a vacuum thermocouple meter 7, an oxygen cylinder 8, a pressure reducing valve I9, a nitrogen cylinder 10, a pressure reducing valve II 11, an oxygen concentration sensor I12, a honeycomb ceramic ring 13, a smoldering reaction chamber 14, a needle valve V15, a needle valve VI 16, a pressure reducing valve III 17, a gas pressure measuring device 18, a gas flow control device 19, a heating device 20, a thermocouple 21, a gas flow indicator 22, an oxygen concentration sensor II 23, a gas pressurizing device 24, a suction type fan 25, a smoke sampling device 26, a mass flowmeter 27, an air bag 28, a pore plate flowmeter 29, a smoldering product collecting tank 30, a push rod I31, a push rod II 32, a filter membrane 33, a filter membrane bracket 34 and.
The synchronous test analysis device for the total smoldering oxygen consumption and the product of the mine reactive polymer material comprises a test gas storage tank 6, a smoldering reaction chamber for placing a cured body of the mine reactive polymer material and a smoldering product collecting tank connected to the gas outlet side of the smoldering reaction chamber, an oxygen cylinder 8 with a pressure reducing valve I9 and a needle valve I1 and a nitrogen cylinder 10 with a pressure reducing valve II 11 and a needle valve II 2 are connected to the test gas storage tank 30 through pipelines, an oxygen concentration sensor I12 is further installed on the test gas storage tank 30, and a vacuum thermocouple meter 7 is installed on the test gas storage tank. An exhaust pump 5 with a needle valve III 3 is installed on the smoldering reaction chamber, and the test gas reservoir tank is communicated with a connecting pipeline of the smoldering reaction chamber through a needle valve IV 4.
The mine reaction type high polymer material solidified body is externally coated with a honeycomb ceramic ring 13, a smoldering reaction chamber 14 is internally provided with a heating device 20 which heats the mine reaction type high polymer material solidified body and is controlled by a computer and a thermocouple 21 which is convenient for testing the temperature change of different positions of the mine reaction type high polymer material solidified body, a test gas storage tank is communicated with the mine reaction type high polymer material solidified body through a pipeline with a gas pressure measuring device 18 and a gas flow control device 19, a pore plate flowmeter 29 with a gas flow indicator 22 is arranged on a connecting pipeline of the smoldering product collection tank and the smoldering reaction chamber, an oxygen concentration sensor II and a needle valve V15 for controlling the communication of a smoldering product collecting tank and a smoldering reaction chamber, wherein a draw-out type fan 25 is installed on a pipeline on the left side of the oxygen concentration sensor II 23, and a gas pressurizing device 24 is installed on a pipeline on the right side of the oxygen concentration sensor II. And a smoke sampling device 26, a mass flow meter 27, an air bag 28 and a needle valve VI 16 are also arranged on a pipeline between the smoldering product collecting tank and the oxygen concentration sensor II.
The invention provides a synchronous experimental analysis method for oxygen consumption and products in the whole smoldering process of a mine reactive polymer material, which comprises the following steps:
s1: closing a needle valve I on an oxygen cylinder 8, a needle valve II on a nitrogen cylinder 10 and a needle valve III on an exhaust pipeline of a smoldering reaction chamber, opening a needle valve IV on a connecting pipeline of a test gas storage tank and the smoldering reaction chamber, simultaneously opening an exhaust pump to carry out vacuum degassing on the test gas storage tank and an air inlet pipeline for distributing air until the reading of a vacuum thermocouple meter arranged on the test gas storage tank is less than or equal to 20, and closing the needle valve IV and the exhaust pump;
step S1 specifically includes the following steps:
s11: closing the needle valve I1, the needle valve II 2 and the needle valve III 3, opening the needle valve IV 4, and starting the exhaust pump 5 to carry out vacuum degassing on the test gas storage tank 6 so as to eliminate the influence of residual air of an air inlet pipeline of gas distribution and the test gas storage tank on a test result in the assembling process of the test device;
s12: the vacuum thermocouple meter 7 arranged on the test gas storage tank is an instrument for monitoring the gas pressure in the test gas storage tank, after the exhaust pump 5 is started to degas the gas inlet pipeline of the gas distribution and the test gas storage tank, if the index of the vacuum thermocouple meter is less than or equal to 20, the gas inlet pipeline of the gas distribution and the test gas storage tank are close to vacuum, and the test requirements are met;
s13: and closing the needle valve IV and the exhaust pump, and stopping degassing the gas inlet pipeline of the gas distribution and the test gas storage tank.
S2: opening a needle valve I and a needle valve II, opening a pressure reducing valve I on an oxygen cylinder and a pressure reducing valve II on a nitrogen cylinder, and configuring test gas in a test gas storage tank to enable the numerical value of an oxygen concentration sensor I to meet the experimental requirements; if the readings of the oxygen concentration sensor I on the test gas storage tank are the values required by the test, closing the needle valve I, the needle valve II, the pressure reducing valve I9 and the pressure reducing valve II 11; if the index of an oxygen concentration sensor I on the test gas storage tank does not reach the numerical value required by the test, closing a needle valve I, a needle valve II, a pressure reducing valve I and a pressure reducing valve II, opening a needle valve IV, starting an exhaust pump to exhaust the test gas storage tank, then closing the needle valve IV and the exhaust pump, opening the needle valve I, the needle valve II, the pressure reducing valve I and the pressure reducing valve II again, and configuring the test gas for the test gas storage tank until the numerical value of the oxygen concentration sensor I meets the experimental requirement;
step S2 specifically includes the following steps:
s21: configuring test gas for the test gas storage tank to enable the value of an oxygen concentration sensor I to meet the experimental requirements, wherein the configuration is carried out according to the oxygen concentration of the mine reactive polymer material in the underground coal mine application environment, and the configured oxygen concentration needs to be consistent with the oxygen concentration value of the mine reactive polymer material in the underground coal mine application environment;
s22: when the test gas is configured, attention should be paid to observing the indication number of the oxygen concentration sensor I on the test gas storage tank, and if the value meets the test requirement, the configuration of the test gas can be stopped;
s23: when the test gas is configured, if the index of the oxygen concentration sensor I on the test gas storage tank is lower than the numerical value required by the test, the pressure reducing valve II and the needle valve II on the high-pressure nitrogen bottle can be closed, the pressure reducing valve I and the needle valve I on the high-pressure oxygen bottle are continuously kept open, the high-pressure oxygen is continuously injected into the test gas storage tank, and the index C of the oxygen concentration sensor I on the to-be-tested gas storage tank1After the test requirements are met, the configuration of the test gas can be stopped;
s24: when the test gas is supplied, if the indication C of the oxygen concentration sensor I on the test gas storage tank1And if the value is higher than the numerical value required by the test, closing a pressure reducing valve II and a needle valve II on the high-pressure nitrogen cylinder, closing a pressure reducing valve I and a needle valve I on the high-pressure oxygen cylinder, opening an exhaust pump to exhaust the test gas storage tank, then closing a needle valve IV and the exhaust pump, opening the needle valve I, the needle valve II, the pressure reducing valve I on the oxygen cylinder and the pressure reducing valve II on the nitrogen cylinder again, and configuring the test gas for the test gas storage tank until the numerical value of the oxygen concentration sensor meets the requirement of the test.
S3: placing the mine reaction type high polymer material solidified body formed after solidification in a honeycomb ceramic ring, and then placing the honeycomb ceramic ring in a smoldering reaction chamber; opening a needle valve III, closing a needle valve V between a smoldering product collecting tank and a smoldering reaction chamber and a needle valve VI between a smoke sampling device and an air bag, and opening an exhaust pump to exhaust the smoldering reaction chamber, an air outlet pipeline of the smoldering reaction chamber and the smoldering product collecting tank; then opening the needle valve V and the needle valve VI, and opening the needle valve III; adjusting a pressure reducing valve III 17 between the test gas storage tank and the smoldering reaction chamber to enable the test gas in the test gas storage tank to flow out, and monitoring the pressure of the test gas through a gas pressure measuring device to enable the value of the pressure to be slightly higher than 0.1 MPa; and simultaneously adjusting the gas flow control device to enable the flow of the test gas to reach the numerical value required by the test;
step S3 specifically includes the following steps:
s31: the mine reaction type high polymer material solidified body is formed by pouring two chemical solutions into a specific mould according to the actual application requirements of the underground coal mine, wherein the mould is a plastic drum with the same inner diameter and height as the honeycomb ceramic ring; the honeycomb ceramic ring wall is hollow, and openings are formed in the inner wall and the outer wall, so that a flowing channel is provided for test gas, and the test gas is in contact with the outer surface of the mining reaction type high polymer material curing body; after the mine reactive polymer material is fully reacted, immediately forming a corresponding solidified body, then removing the die by using a blade, and placing the mine reactive polymer material solidified body in the honeycomb ceramic ring; then placing the honeycomb ceramic ring with the mine reaction type high polymer material solidified body into a smoldering reaction chamber;
s32: the smoldering reaction chamber has an outer wall made of stainless steel and an inner wall made of nano microporous material, and has the functions of providing space for the smoldering chemical reaction of the mine reactive high polymer material and preventing the smoldering process from being influenced by the external temperature; one end of the smoldering reaction chamber is provided with a flange which is matched with a flange on the heating device to realize connection; the flange is provided with bolt holes, and the flange is fastened by bolts during connection; the end faces of the flanges are provided with circular grooves, and high-temperature-resistant rubber rings are placed in the circular grooves when the flanges are connected, so that the end faces of the two flanges are sealed, the gas in a smoldering reaction chamber is prevented from leaking, and the reliability of a test result is ensured; the heating device is used for heating the mine reaction type high polymer material solidified body, and the starting and heating rates of the heating device are controlled by a computer connected with the heating device;
s33: opening the needle valve III, closing the needle valve V and the needle valve VI, and opening an exhaust pump to exhaust the smoldering reaction chamber, the gas outlet pipeline of the smoldering reaction chamber and the smoldering product collecting tank so as to eliminate the influence of external air entering the smoldering reaction chamber, the gas outlet pipeline of the smoldering reaction chamber and the smoldering product collecting tank on the test result in the assembling process of the test device and the mine reaction type high polymer material solidified body test piece; the inner walls of the gas outlet pipeline of the smoldering reaction chamber and the smoldering product collecting tank are both sprayed with nano materials, and the function of the nano materials is to ensure that smoke generated in the test process is not adsorbed on the inner walls of the gas outlet pipeline of the smoldering reaction chamber and the smoldering product collecting tank;
s34: the pressure reducing valve III on the test gas storage tank enables the test gas in the test gas storage tank to flow out, the pressure of the test gas is monitored through the gas pressure measuring device, the numerical value of the pressure is slightly higher than 0.1MPa, the test gas in the test gas storage tank flows out through adjusting the pressure reducing valve III, and the pressure of the flowing-out test gas can be monitored through the gas pressure measuring device; because the space atmospheric pressure applied by the mine underground reactive polymer material is close to 0.1MPa, when the extraction type fan arranged on the gas outlet side of the smoldering reaction chamber operates, a certain pressure difference is generated to enable the test gas to flow in the smoldering reaction chamber and the pipeline, the pressure of the flowing-out test gas is required to be ensured to be slightly higher than 0.1MPa, and therefore the pressure of the test gas contacting with the mine reactive polymer material test piece in the smoldering reaction chamber is close to the underground atmospheric pressure of the coal mine;
s35: simultaneously adjusting the gas flow control device to make the flow of the test gas reach the value required by the test, and defining the value as VjThe value V ofjThe method is characterized in that the flow of the test gas flowing out of the test gas storage tank is adjusted according to the flow velocity of the wind flow in the working condition environment of the mine reactive polymer material used in the underground coal mine, so that the mine reactive polymer material solidified body in the smoldering reaction chamber is testedThe flow speed of the test gas contacted by the piece is equal to or close to the wind flow speed in the actual working condition environment.
S4: starting a heating device to heat the mine reaction type high polymer material solidified body, and adjusting the heating rate according to the test requirement; meanwhile, starting a thermocouple, a gas flow indicator, an oxygen concentration sensor II, a gas pressurizing device and a draw-out fan;
step S4 specifically includes the following steps:
s41: the heating device is controlled by a computer, and the heating rate of the heating device can be adjusted and controlled by the computer to meet the requirements of a test scheme;
s42: the thermocouple is inserted into the interior of the mine reaction type high polymer material solidified body and is used for measuring the change of the internal temperature field of the mine reaction type high polymer material solidified body in the smoldering test process, the measured temperature data is transmitted to the computer, and the temperature change of different positions in the mine reaction type high polymer material solidified body at different time in the whole smoldering test process is obtained through data processing;
s43: the gas flow indicator is connected to the gas inlet side and the gas outlet side of the orifice plate flowmeter through a pressure measuring pipeline, and the flow Vc of the test gas after passing through the mine reactive polymer material solidified body can be obtained by calculating the gas pressure difference between the two ends of the gas inlet side and the gas outlet side of the orifice plate flowmeter; the straight pipe section on the air inlet side of the orifice plate flowmeter is more than or equal to 10 times of the inner diameter of the pipeline, and the straight pipe section on the air outlet side of the orifice plate flowmeter is more than or equal to 5 times of the inner diameter of the pipeline; the oxygen concentration sensor II is used for monitoring the oxygen concentration value C of the test gas in the pipeline after the test gas passes through the mine reaction type high polymer material solidified body2;
S44: the gas pressurizing device is used for pressurizing and conveying the gas passing through the mine reaction type high polymer material solidified body into the smoldering product collecting tank, and the volume of the smoldering product collecting tank is Vs;
S45: the surfaces of the blades and the flow channel of the draw-out fan are sprayed with nano materials, and the effect of the nano materials is to prevent smoke generated in the smoldering test process from being attached to the surfaces of the blades and the flow channel of the draw-out fan, so that the influence on the final calculation of the smoke yield in the whole smoldering process is caused.
S5: in the test process, sampling the smoke in the pipeline through a smoke sampling device arranged on the pipeline at intervals according to the test requirements; opening the needle valve VI and the mass flowmeter while sampling the smoke, enabling part of gas after smoldering reaction to enter the air bag, simultaneously recording the readings of a gas flow indicator connected with the orifice plate flowmeter and the readings of an oxygen concentration sensor II, and controlling the sampling time within 60 s;
step S5 specifically includes the following steps:
s51: the smoke sampling device is connected with an air outlet pipeline of the smoldering reaction chamber through a flange; the sampling device consists of a short-circuit pipeline and a sampling device with the upper part as shown in figure 2; the inner diameter and the outer diameter of the short-circuit pipeline are the same as those of the gas outlet pipeline of the smoldering reaction chamber; the quarter circular arc part of the short-circuit pipeline is connected with the pipeline through a hinge structure, the quarter circular arc part of the short-circuit pipeline is connected with a push rod II 32 in the sampling device at the upper part through an iron wire, the push rod II is of a piston structure, and when the push rod II is pulled outwards, the quarter circular arc part of the short-circuit pipeline is separated from the short-circuit pipeline; the part of the short-circuit pipeline, the top of which is contacted with the quarter-arc part, adopts the magnet 35, and when sampling is not needed, the magnet attracts the quarter-arc part to prevent gas in the pipeline from leaking; when sampling, pulling the push rod II to separate the quarter arc part of the short-circuit pipeline from the short-circuit pipeline, and then pushing the push rod I31 downwards to drive the filter membrane bracket to move to the quarter arc part of the original short-circuit pipeline; the filter membrane bracket is made of plastic, and the outer surface of the filter membrane bracket is sprayed with nano materials to prevent smoke from attaching to the filter membrane bracket; a filter membrane 33 is further arranged on the filter membrane bracket 34, and the area of the filter membrane is equal to one fourth of the area of the inner section of the pipeline;
s52: when sampling, recording the time t for starting samplingqAfter 60s, pulling the push rod I to take out the filter membrane, and then pushing the push rod II to connect the quarter circular arc part of the short-circuit pipeline with the short-circuit pipeline;
s53: opening the needle valve VI and the mass flowmeter during sampling to ensure that part of gas after smoldering reaction enters the air bag, and recording the accumulated flow in the sampling period of 60s as Vqt(ii) a And simultaneously recording the indication Vc of a gas flow indicator connected with the orifice plate flowmeter and the indication C of an oxygen concentration sensor II2t。
S6: when the reading of the oxygen concentration sensor II is equal to that of the oxygen concentration sensor I, closing the heating device, the pressure reducing valve III, the gas flow control device, the gas flow indicator, the extraction type fan, the gas pressurizing device, the needle valve V and the mass flow meter;
step S6 specifically includes the following steps:
s61: when the indication of the oxygen concentration sensor II is equal to the indication of the oxygen concentration sensor I, the oxygen concentration in the test gas entering the smoldering reaction chamber is equal to the oxygen concentration in the gas flowing out of the smoldering reaction chamber, namely the smoldering reaction of the mine reactive polymer material solidified body does not consume oxygen, and the smoldering process can be considered to be finished;
s62: and when the smoldering process is finished, stopping sampling operation, and immediately closing the heating device, the pressure reducing valve III, the gas flow control device, the gas flow indicator, the extraction type fan, the gas pressurizing device, the needle valve V and the mass flow meter.
S7: weighing the smoke sample obtained each time, and obtaining the obtained smoke mass, which is recorded as myt(ii) a Then, the smoke yield within the corresponding sampling time 60s can be obtained; obtaining the smoke generation rate at the corresponding moment in the test process, drawing a curve of the smoke generation rate changing along with time, obtaining a polynomial expression of the curve of the smoke generation rate changing along with time by adopting a polynomial fitting method, and then obtaining the accumulated smoke yield in the test process by adopting an integration method;
step S7 specifically includes the following steps:
s71: the mass of the filter membrane before and after sampling was weighed to obtain the mass 4m of the smoke generated within 60s of the samplingytThe generating speed of the smoke is 4m in the smoldering process of the mine reaction type high polymer material solidified bodyyt/min;
S72: then the cigarettes with different sampling times obtained in the whole test process are sampledGeneration rate m of mistytAnd/min, drawing a corresponding curve changing along with time, obtaining a polynomial expression of the curve changing along with time of the smoke generation rate by adopting a polynomial fitting method, and marking as: f (m)yt);
S73: the obtained polynomial expression f (m)
yt) Determining the duration t of the entire smoldering test procedure
zThe integration of (1):
i.e. the cumulative smoke yield during the test.
S8: multiplying the readings of the oxygen concentration sensor I and the oxygen concentration sensor II in each sampling by the readings of the gas flow control device and the readings of the gas flow indicator arranged on the orifice plate flowmeter respectively, and obtaining the smoldering oxygen consumption speed of the mine reaction type high polymer material solidified body corresponding to each sampling through data processing; then drawing a curve of smoldering oxygen consumption speed of the mine reaction type high polymer material solidified body changing along with time, obtaining a polynomial expression of the curve of smoldering oxygen consumption speed of the mine reaction type high polymer material solidified body changing along with time by adopting a polynomial fitting method, and then obtaining accumulated oxygen consumption in the test process by adopting an integration method;
step S8 specifically includes the following steps:
s81: will (V)j×C1-Vc×C2) The oxygen consumption speed h of smoldering of the mine reaction type high polymer material solidified body in each sampling can be calculatedtDimension of m3Min; then drawing a curve of smoldering oxygen consumption speed of the mine reaction type high polymer material solidified body changing along with time, and obtaining a polynomial expression lambda (h) of the curve of smoldering oxygen consumption speed of the mine reaction type high polymer material solidified body changing along with time by adopting a polynomial fitting methodt);
S82: the polynomial expression λ (h) to be obtained
t) Determining the duration t of the entire smoldering test procedure
zThe integration of (1):
namely the accumulated smoldering oxygen consumption of the mine reaction type high polymer material solidified body in the test process.
S9: performing component analysis on the gas collected in the air bag each time by using a gas chromatography analysis method to obtain the concentration of corresponding combustible or harmful gas; multiplying the numerical value by the index of the mass flowmeter to obtain the output rate of the combustible or harmful gas within the corresponding sampling time of 60s, then drawing a curve of the output rate and speed of the combustible or harmful gas changing along with time, obtaining a polynomial expression of the curve of the output rate of the combustible or harmful gas changing along with time by adopting a polynomial fitting method, and then obtaining the quantity of the combustible or harmful gas in the test process by adopting an integral method;
step S9 specifically includes the following steps:
s91: the air bag is connected with a gas chromatography device, and the concentration of corresponding combustible or harmful gas C can be obtained through analysisqtAnd multiplying the value by the reading M of the mass flow meterqtNamely: (C)qt×Mqt) The output rate of combustible or harmful gas within 60s of corresponding sampling time is (C)qt×Mqt)/min;
S92: then the generation rate of combustible or harmful gas at different sampling time obtained in the whole test process is (C)qt×Mqt) And/min, drawing a corresponding curve changing along with time, obtaining a polynomial expression of the curve changing along with the time t of the generation rate of the combustible or harmful gas by adopting a polynomial fitting method, and marking as: ψ (t);
s93: the obtained polynomial expression psi (t) is used for calculating the duration t of the whole smoldering test process
zThe integration of (1):
i.e. the cumulative amount of combustible or hazardous gas produced during the test.
The invention discloses a synchronous test analysis device and a synchronous test analysis method for oxygen consumption and products of a mine reactive high polymer material smoldering process, and aims to obtain the oxygen consumption, the smoke output rate and the combustible and harmful gas output rate of a mine reactive high polymer material solidified body under different time conditions in the smoldering test process, and further obtain the oxygen consumption, the smoke, the combustible and the harmful gas accumulated output in the whole smoldering process.
The specific method comprises the following steps: placing the mine reaction type high polymer material solidified body in a honeycomb ceramic ring, then placing the honeycomb ceramic ring into a smoldering reaction chamber, and heating the mine reaction type high polymer material solidified body by a heating device controlled by a computer; opening a test gas storage tank while heating, controlling the gas flow contacted with the mine reactive polymer material solidified body through a gas flow control device, and truly simulating the gas flow velocity in different application environments under the coal mine; the temperature change of different positions in the mine reactive polymer material solidified body under different time conditions in the smoldering process is tested by the arranged thermocouple. In the smoldering test process, the gas flow at the gas outlet side of the smoldering reaction chamber is measured by a pore plate flowmeter, the values acquired by the oxygen concentration sensor I and the oxygen concentration sensor II are combined, and the oxygen concentration of the prepared test gas and the flow controlled by the gas flow control device are compared, so that the oxygen consumption rate of the mine reaction type high polymer material solidified body in the smoldering process can be obtained; and further fitting a curve of the oxygen consumption rate changing along with the smoldering time to obtain a corresponding fitting polynomial, and integrating the polynomial to obtain the accumulated oxygen consumption of the mine reactive high polymer material solidified body in the smoldering process.
In the process of the smoldering test, the smoke output rate of any smoldering time can be obtained through the smoke sampling device, the corresponding fitting polynomial is obtained through fitting of a curve of the smoke output rate changing along with the smoldering time, and the accumulated smoke output of the ore reaction type high polymer material solidified body in the smoldering process can be obtained through integration of the polynomial.
In the process of smoldering test, the combustible and harmful gas output rate in any smoldering time can be obtained by a method of combining a mass flow meter, an air bag and gas chromatography, a corresponding fitting polynomial is obtained by fitting a curve of the combustible and harmful gas output rate changing along with the smoldering time, and the accumulated combustible and harmful gas output quantity of the mine reaction type high polymer material solidified body in the smoldering process can be obtained by integrating the polynomial.
Finally, it is noted that the above-mentioned preferred embodiments illustrate rather than limit the invention, and that, although the invention has been described in detail with reference to the above-mentioned preferred embodiments, it will be understood by those skilled in the art that various changes in form and detail may be made therein without departing from the scope of the invention as defined by the appended claims.