CN105510175A - Method for measuring inhibition performance of inhibitor - Google Patents
Method for measuring inhibition performance of inhibitor Download PDFInfo
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- CN105510175A CN105510175A CN201510900388.5A CN201510900388A CN105510175A CN 105510175 A CN105510175 A CN 105510175A CN 201510900388 A CN201510900388 A CN 201510900388A CN 105510175 A CN105510175 A CN 105510175A
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- G01N7/00—Analysing materials by measuring the pressure or volume of a gas or vapour
- G01N7/02—Analysing materials by measuring the pressure or volume of a gas or vapour by absorption, adsorption, or combustion of components and measurement of the change in pressure or volume of the remainder
- G01N7/04—Analysing materials by measuring the pressure or volume of a gas or vapour by absorption, adsorption, or combustion of components and measurement of the change in pressure or volume of the remainder by absorption or adsorption alone
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N7/00—Analysing materials by measuring the pressure or volume of a gas or vapour
- G01N7/14—Analysing materials by measuring the pressure or volume of a gas or vapour by allowing the material to emit a gas or vapour, e.g. water vapour, and measuring a pressure or volume difference
- G01N7/18—Analysing materials by measuring the pressure or volume of a gas or vapour by allowing the material to emit a gas or vapour, e.g. water vapour, and measuring a pressure or volume difference by allowing the material to react
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Abstract
The invention belongs to the technical field of underground coal spontaneous combustion disaster prevention and treatment of a coal mine, and particularly relates to a method for measuring the inhibition performance of an inhibitor. According to the adsorbing capacity difference of oxygen before and after the inhibitor is added into a coal sample, an inhibition rate E1 of the inhibitor on oxygen absorption is calculated, a CO volume concentration difference generated before and after the inhibitor is added into the coal ample is checked to calculate an inhibition rate E2 on the oxygen after the spontaneous combustion of the coal sample, and the inhibition rate E1 and the inhibition rate E2 are combined to analyze and obtain the inhibition performance of the inhibitor in the whole coal sample spontaneous combustion process. The method disclosed by the invention is combined with the traditional method, and can be used for investigating an inerting function performed by the inhibitor in the whole coal sample spontaneous combustion oxidation process, the one-sidedness of a traditional inhibition performance metering method is changed, by combining the method with the traditional inhibition performance measurement method, the inhibition efficiency of the inhibitor can be more scientifically and reasonably determined, and a new method is provided for selecting the inhibitor in coal mine fire preventing and extinguishing technical work.
Description
Technical field
The invention belongs to underground coal mine control coal spontaneous combustion disaster technical field, particularly a kind of method measuring retarder resistance voltinism energy.
Background technology
China's coal-mine Conflagration Caused by Coal Self-ignition accident is very serious, and wherein heterogeneous goaf is up to about 60% of spontaneous fire, and the fat coal loss amount caused due to coal spontaneous combustion is huge.Spontaneous combustion of coal has not only burnt valuable resource, produces a large amount of CO, CO
2and SO
2deng toxic and harmful, the health and lives of harm workman, contaminated environment; Can also bring out the generation of gas, dust explosion accident, be the disaster hindering Safety of Coal Mine Production.
The oxidation and spontaneous combustion of coal is from physisorption oxygen under coal low temperature.Because coal is a kind of porous material, under normal temperature and pressure conditions, oxygen molecule produces physisorption in the aperture of coal, and physical adsorption process is the process of a heat release, but the heat of adsorption of releasing is less.Along with the carrying out of absorption, in oxygen and coal there is chemisorption in functional group pendant, a large amount of chemisorption heat is released, if these heats have little time to be discharged in air, the temperature of coal body will be made to increase, temperature rising can aggravate the carrying out of chemical reaction, finally causes colliery to occur spontaneous combustion phenomenon.
The preventing and extinguishing fire technologies such as at present comparatively conventional suppression spontaneous combustion of coal method has water filling, is in the milk, shutoff of leaking out, retarder, all pressure, inert gas, gel.Wherein retarder preventing and extinguishing fire technology is widely applied in suppression spontaneous combustion of coal, and obtain good result, retarder has number of different types, comprises halogen retarder, ammonium salt retarder, bases retarder, gel retardant, anti-oxidant class retarder, compound retarder and foam retarder etc.
At present, in " Coal Mine Fire retarder general technical specifications ", the method for testing of regulation retarder resistance voltinism energy is under specific experimental conditions, the number percent of the CO volumetric concentration that the difference of the CO volumetric concentration that inspection raw coal sample and resistanceization coal sample produce and raw coal sample produce, that is:
E=（A-B）/A*100；
E in formula---resistance rate, %;
When A---coal sample processes without resistanceization, the concentration of the CO released when passing into purge drying air (160mL/min) in temperature rise (100 DEG C) test, 10
-6;
B---coal sample through resistanceization process after, the concentration of the CO released under above-mentioned the same terms, 10
-6.
In the definition of resistance rate, using 100 DEG C as standard temperature when measuring, there is certain weak point in this method: the first, and in 100 DEG C of situations, under aerobic environment, oxidation of coal release CO generation is along with time increase; The second, retarder is not only work at a certain temperature to coal spontaneous combustion resistanceization, but has Inhibition to whole Coal Self-ignition Process, and is not identical in its resistanceization effect of different temperatures and time period with playing the mechanism of Inhibition.
Another kind of method of testing is in the temperature programmed oxidation process of coal, the difference detecting raw coal sample and the temperature of resistanceization coal sample sometime with this to determine the resistance voltinism energy of retarder.The weak point of this method is tested identical with above-mentioned resistance rate, and coal sample temperature contrast sometime can not represent the resistance effect of retarder in whole Coal Self-ignition Process.
Summary of the invention
For the deficiency that existing method of testing exists, the invention provides a kind of method measuring retarder resistance voltinism energy, object is the Inhibition according to coal adsorption of oxygen process, in conjunction with existing resistance rate method of testing, judge that retarder is to control Coal Self-ignition Process role better, thus more comprehensively judge the resistance effect of retarder.
The technical scheme realizing the object of the invention is carried out according to following steps:
(1) coal sample chosen is processed as coal dust, put into the adsorbing cylinder of coal adsorption of oxygen pick-up unit, in adsorbing cylinder, remaining space is full of air, air ambient during spontaneous combustion of simulated coal, adsorbing cylinder is equipped with gas vent and tensimeter, gas vent is connected with gas chromatograph, and according to oxygen concentration in adsorbing cylinder before and after absorption and pressure change, under measuring normal temperature and pressure conditions, coal is to the adsorbance A of oxygen in air;
(2) retarder solution is prepared, it is mixed according to a certain percentage with coal sample, put into adsorbing cylinder after drying, add the coal after retarder under measuring normal temperature and pressure conditions to the adsorbance B of oxygen in air, add before and after retarder that according to coal sample resistance rate E is calculated to the difference of the adsorbance of oxygen
1, wherein E
1=(A-B)/A*100;
(3) the retarder solution that preparation is identical with step (2), according to the method for testing of the retarder resistance voltinism energy of regulation in " Coal Mine Fire retarder general technical specifications ", inspection coal sample, in the difference of adding the CO volumetric concentration produced before and after retarder, calculates resistance rate E
2;
(4) E in step (2)
1be before coal sample spontaneous combustion retarder to the resistance efficiency of oxygen, the E in step (3)
2be the resistance efficiency to oxygen after coal sample spontaneous combustion, the two combines analysis, obtains the resistance voltinism energy of this retarder in whole coal sample spontaneous combustion process.
Compared with prior art, feature of the present invention and beneficial effect are:
Retarder inerting effect to oxidation of coal in the heating and oxidation process of coal has been investigated with the rate method of CO generation mensuration resistanceization in prior art, the method of mensuration retarder group voltinism energy of the present invention has then investigated the impact of retarder on coal physisorption oxygen by the change detection resistance rate of coal on Oxygen Adsorption amount, the first step due to oxidation and spontaneous combustion is exactly that coal is to oxygen generation physical and chemical adsorption, therefore the Inhibition of retarder to coal adsorption of oxygen is judged by this method, again in conjunction with the resistance rate to the inerting effect of oxidation of coal in the heating and oxidation process of coal of retarder in prior art, based on the inventive method, when choosing retarder, first the first step that can suppress coal oxidation should be chosen---the retarder of coal adsorption of oxygen effect, secondly select in the Temperature Programmed Processes of coal, the retarder that coal generation oxidation and spontaneous combustion reacts can be suppressed, make retarder to choose science more comprehensive, there is Social benefit and economic benefit widely.
The inventive method is combined with classic method, can investigate retarder in whole coal spontaneous combustion oxidizing process the inerting effect that plays, change the unilateral of conventional metered dose resistanceization performance methodology, the method hindering voltinism energy with traditional measurement combines, the resistance efficiency of determination retarder that can be more scientific and reasonable, for choosing of retarder in preventing and extinguishing fire of coal mine technical work provides a kind of new method.
Accompanying drawing explanation
Fig. 1 is coal adsorption of oxygen pick-up unit schematic diagram of the present invention;
Wherein 1: adsorbing cylinder; 2: gas chromatograph; 3: tensimeter; 4: gas vent;
Fig. 2 is the functional group's change infrared spectrogram after the independent coal sample adsorption of oxygen in the embodiment of the present invention;
Fig. 3 is functional group's change infrared spectrogram before and after the coal sample adsorption of oxygen after the interpolation retarder in the embodiment of the present invention.
Embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is described further.
The present embodiment chooses peaceful upper strata, vertical ore deposit, Haizhou, Fuxin coal sample.
The method of the mensuration retarder resistance voltinism energy of the present embodiment, carry out according to following steps:
(1) coal sample chosen is passed through fragmentation, grinding, screening, be processed as the following coal dust of 50 order, take the adsorbing cylinder 1 that 1Kg coal dust puts into coal adsorption of oxygen pick-up unit, the structure of coal adsorption of oxygen pick-up unit as shown in Figure 1, in adsorbing cylinder 1, remaining space is full of air, air ambient during spontaneous combustion of simulated coal, adsorbing cylinder 1 is equipped with gas vent 4 and tensimeter 3, gas vent 4 is connected with gas chromatograph 2, according to oxygen concentration in adsorbing cylinder before and after absorption and pressure change, under mensuration normal temperature and pressure conditions, 1kg coal is 4.79L to the adsorbance of oxygen in air;
Adopt the change of Mei Zhong functional group before and after infrared spectrum measurement absorption, as shown in Figure 2, CH in coal before and after discovery absorption
2, CH
3functional group is changed significantly;
(2) preparing mass concentration is the MgCl of 20%
2retarder solution, mixes it according to mass ratio 4:1 with 1kg coal sample, leaves standstill 12h after stirring, then 40 DEG C of dryings 24 hours in vacuum drying chamber, puts into adsorbing cylinder, adds MgCl under measuring normal temperature and pressure conditions
2coal after retarder is 2.05L to the adsorbance of oxygen in air, adds before and after retarder calculating resistance rate E to the difference of the adsorbance of oxygen according to coal sample
1, wherein E
1=(4.79-2.05)/4.79*100=57.2%;
Adopt the change adding the Mei Zhong functional group of retarder before and after infrared spectrum measurement absorption, as shown in Figure 3, CH in coal before and after discovery absorption
2, CH
3functional group's amplitude of variation is less than the coal sample of not adding retarder, illustrates that the retarder in the present embodiment can make coal inerting, reduces speed and the quantity of coal adsorption of oxygen, thus stops the carrying out of coal spontaneous oxidation;
(3) adopt water-bath temperature programme spontaneous combustion of simulated coal process, utilizing the resistance rate assay method of the CO generation of regulation in " Coal Mine Fire retarder general technical specifications " to record resistance rate is E
2be 51.5%
Although the resistance rate numerical value measured by above-mentioned two kinds of methods disagrees, method of testing is different, therefore can not mutually compare.The resistance rate assay method of CO generation has investigated retarder inerting effect to oxidation of coal in the heating and oxidation process of coal, and the resistance rate assay method of coal on Oxygen Adsorption amount has investigated the impact of retarder on coal physisorption oxygen, can see in the present embodiment, by MgCl
2coal sample after process, it is more weak than the ability of untreated coal sample adsorption of oxygen to the adsorptive power of oxygen, and adsorbance reduces, the first step due to oxidation and spontaneous combustion be exactly coal to oxygen generation physical and chemical adsorption, therefore judge the Inhibition of retarder to coal adsorption of oxygen by this method.In addition, this experimental technique is combined with classic method, can investigate retarder in whole coal spontaneous combustion oxidizing process the inerting effect that plays.
Claims (2)
1. measure a method for retarder resistance voltinism energy, it is characterized in that carrying out according to following steps:
(1) coal sample chosen is processed as coal dust, put into the adsorbing cylinder of coal adsorption of oxygen pick-up unit, in adsorbing cylinder, remaining space is full of air, air ambient during spontaneous combustion of simulated coal, according to oxygen concentration in adsorbing cylinder before and after absorption and pressure change, under measuring normal temperature and pressure conditions, coal is to the adsorbance A of oxygen in air;
(2) retarder solution is prepared, it is mixed according to a certain percentage with coal sample, put into adsorbing cylinder after drying, add the coal after retarder under measuring normal temperature and pressure conditions to the adsorbance B of oxygen in air, add before and after retarder that according to coal sample resistance rate E is calculated to the difference of the adsorbance of oxygen
1, wherein E
1=(A-B)/A*100;
(3) the retarder solution that preparation is identical with step (2), according to the method for testing of the retarder resistance voltinism energy of regulation in " Coal Mine Fire retarder general technical specifications ", inspection coal sample, in the difference of adding the CO volumetric concentration produced before and after retarder, calculates resistance rate E
2;
(4) E in step (2)
1be before coal sample spontaneous combustion retarder to the resistance efficiency of oxygen, the E in step (3)
2be the resistance efficiency to oxygen after coal sample spontaneous combustion, the two combines analysis, obtains the resistance voltinism energy of this retarder in whole coal sample spontaneous combustion process.
2. a kind of method measuring retarder resistance voltinism energy according to claim 1, it is characterized in that described adsorbing cylinder is equipped with gas vent and tensimeter, gas vent is connected with gas chromatograph.
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| CN201510900388.5A CN105510175B (en) | 2015-12-08 | 2015-12-08 | A kind of method for determining retardant resistanceization performance |
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| CN201510900388.5A CN105510175B (en) | 2015-12-08 | 2015-12-08 | A kind of method for determining retardant resistanceization performance |
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| CN105510175B CN105510175B (en) | 2018-04-06 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113218774A (en) * | 2021-04-15 | 2021-08-06 | 中国矿业大学 | Mining microcapsule stopping agent compressive strength test system and test method |
| CN114113454A (en) * | 2021-11-08 | 2022-03-01 | 太原工业学院 | Testing device and method for testing effect of stopping agent |
Citations (5)
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| EP0069393A1 (en) * | 1981-07-08 | 1983-01-12 | Rheinische Braunkohlenwerke AG. | Method for the early detection of carbonic fires in recipients containing dust of brown coal by detection of methane |
| CN101000333A (en) * | 2006-12-19 | 2007-07-18 | 煤炭科学研究总院重庆分院 | Device for investigating coal self-combustion tendentiousness based on low temp oxidation oxygen consumption |
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2015
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| EP0069393A1 (en) * | 1981-07-08 | 1983-01-12 | Rheinische Braunkohlenwerke AG. | Method for the early detection of carbonic fires in recipients containing dust of brown coal by detection of methane |
| CN101000333A (en) * | 2006-12-19 | 2007-07-18 | 煤炭科学研究总院重庆分院 | Device for investigating coal self-combustion tendentiousness based on low temp oxidation oxygen consumption |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113218774A (en) * | 2021-04-15 | 2021-08-06 | 中国矿业大学 | Mining microcapsule stopping agent compressive strength test system and test method |
| CN113218774B (en) * | 2021-04-15 | 2022-04-19 | 中国矿业大学 | Mining microcapsule stopping agent compressive strength test system and test method |
| CN114113454A (en) * | 2021-11-08 | 2022-03-01 | 太原工业学院 | Testing device and method for testing effect of stopping agent |
| CN114113454B (en) * | 2021-11-08 | 2024-03-29 | 太原工业学院 | Device and method for testing effect of inhibitor |
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