CN106706819A - Application of 1,1,1,2-tetrafluoroethane used as tracer in coal mine gas - Google Patents
Application of 1,1,1,2-tetrafluoroethane used as tracer in coal mine gas Download PDFInfo
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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Abstract
The invention relates to the technical field of tracers and provides application of 1,1,1,2-tetrafluoroethane used as a tracer in coal mine gas. The invention disclsoes the application of the 1,1,1,2-tetrafluoroethane used as the tracer in the coal mine gas for the first time; compared with a traditional tracer SF6, the 1,1,1,2-tetrafluoroethane has the advantages of high sensitivity, good stability, less adsorption amount of a coal seam and the like; especially, the detection limit is very low and the lowest detection limit can reach 3*10<-12>mg/m<3>; the 1,1,1,2-tetrafluoroethane has less dosage and low cost and has obvious advantages when being compared with the traditional tracer SF6; and meanwhile, the 1,1,1,2-tetrafluoroethane is environmentally friendly, has small damages to an ozone layer and short residue time, can be rapidly degraded in atmosphere and is used as the tracer and can be applied to the coal mine gas better.
Description
Technical field
The present invention relates to Tracer Technique field, be a kind of HFA 134a as tracer in coal mine gas
Application.
Background technology
China is one of country of coal and gas prominent accident most serious in the world, and mine quantity is more, have a very wide distribution, increase
Speed long is fast, the burst accident many, number of casualties of number is more, super-huge accident is continuous.It is to reduce and prevent coal to take out coal-bed gas in advance
With the important technique measure of Gas Outburst disaster.The rational spacing of wells is the important parameter for influenceing gas pumping effect, drilling
Spacing is excessive, easily forms pumping blind zone, and spacing is too small, easily causes the waste of resource.The arrangement of drilling should be with extraction effectively half
Footpath is foundation, so as to realize optimal extracting result.Therefore, Accurate Determining concordant hole pumping and mining effective radius is pre- to coal-bed gas
Draining borehole arrangement has important directive function.In recent years, tracer technique is to select suitable material to be added to need spike stream
In body, the technology of fluid motion state rule is analyzed by monitoring the change of extraction tracer concentration.A kind of preferable gas shows
Track agent itself will possess detection sensitivity very high, environment-protecting asepsis, harmless, background concentration is low, stable in coal seam
The features such as property is good, adsorption capacity is small in the earth formation.
The application of search gas has history very long, the search gas used in colliery mainly SF6；SF6It is lazy as one kind
Property gas, be at normal temperatures and pressures a kind of colourless, odorless, nontoxic, non-ignitable, free from corrosion gas, generally carry out mine leakage with it
Wind detection, determines coal seam coal gas dynamics state etc..At present, SF is analyzed in mine6Sample mainly captures gas phase color using electronics
Spectrometry and SF6Leak detector etc..
Traditional coal mine gas tracer SF6With following weak point：(1)SF6It is a kind of very strong gas of greenhouse effects
Body, has greater environmental impacts, by SF6During as gas tracer, if passage is revealed, SF6It is easy to be discharged into air and causes
Environmental pollution, causes greenhouse effects, and SF is considered from environmental angle6There are problems that as tracer very big.(2)SF6It is applied to colliery
Tracer has gas residue, the SF of residual under mine6Interference, influence monitoring can be produced for colliery Tracing detection next time
As a result.
HFC-134a is a kind of without chlorine atom, the refrigerant with Good Security.HFC-134a destruction ozone is dived
It is 0 that (ODP) can be worth, and global warming coefficient value (GWP) is that 1300, ASHRAE level of securitys are A1 (nontoxic non-combustible), in air
Middle existence time is very short, and innocuous substance can be completely decomposed into 14.5, is a kind of most popular middle low-temperature environment-friendly system
Cryogen.And SF6Although nontoxic, global warming potential is 23900, and RT is 3200 in an atmosphere；HFC-134a
With good combination property, the substitute of a kind of highly effective and safe traditional freon class refrigerant, mesh are become
Before be mainly used in the field of refrigerant；But relevant 1,1,1,2- HFC-134as applying in coal mine gas as tracer
Report is showed no both at home and abroad, the document of correlation is not retrieved yet.
The content of the invention
A kind of application the invention provides HFA 134a as tracer in coal mine gas, overcomes
The deficiency of prior art is stated, it can effectively solve traditional coal mine gas tracer SF6Not environmentally, monitoring result and is easily influenceed；
Application about 1,1,1,2- HFC-134as as tracer in coal mine gas is at home and abroad showed no the problem of report.
The technical scheme is that realized by following measures：A kind of 1,1,1,2- HFC-134as are used as tracer
Application in coal mine gas.
Application present invention firstly discloses 1,1,1,2- HFC-134as as tracer in coal mine gas；1,1,1,2-
The more traditional tracer SF of HFC-134a6There is sensitivity high, good stability, adsorbance is few in the middle of coal seam, especially
Detection limit is very low, and minimum detectability can reach 3 × 10-12mg/m3, consumption is few, low cost, compared to traditional tracer SF6
There is obvious advantage；HFA 134a environmental protection simultaneously, small to depletion of the ozone layer, the residence time is short, in an atmosphere can be fast
Prompt drop solution, preferably can apply in coal mine gas as tracer.
Brief description of the drawings
Accompanying drawing 1 is 1,1,1,2- HFC-134as and traditional gas tracer SF6Stability comparison diagram in 30 days.
Accompanying drawing 2 is 1,1,1,2- HFC-134as and traditional gas tracer SF6The comparison diagram of uncertainty.
Accompanying drawing 3 is the concentration standard curve of 1,1,1,2- HFC-134as.
Accompanying drawing 4 is that 1,1,1,2- HFC-134as drainage radius influence situation comparison diagram to extraction rate.
Specific embodiment
The present invention is not limited by following embodiments, can technology according to the present invention scheme and actual conditions determine specifically
Implementation method.
Embodiment 1, application of the HFA 134a as tracer in coal mine gas.
The application of the 1,1,1,2- HFC-134as as tracer in coal mine gas is detected by following experiment：
1. the HFA 134a as tracer detection method condition, detecting instrument be gas chromatograph configuration
Electron capture detector or flame ionization ditector；Chromatographic column is DB-5 or same type capillary chromatographic column, chromatographic column
Flow：Constant flow rate 1.5ml/min；Injection port pattern：Do not shunt；Carrier gas：Nitrogen；Post case temperature：90℃；Retention time：
7min。
2. the HFA 134a as tracer stability experiment, HFA 134a and SF6Stand 1
It was to 30 days, and every 5 days of period periodically using its response peak area of gas chromatograph for determination and calculated its concentration, dense by tracer
The Assessment of Changes of degree its stability；1,1,1,2- HFC-134as and traditional gas tracer SF under the same terms6In 30 days
As shown in Figure 1, HFC-134a is the abbreviation of HFA 134a to stability comparison diagram in Fig. 1；It will be seen from figure 1 that
After being stood under same experimental conditions, the relative standard deviation of HFA 134a change in concentration is 1.02%, SF6Concentration becomes
The relative standard deviation of change is 1.4%, illustrates the good stability of HFA 134a in SF6Stability.
3. the HFA 134a is tested as the method for testing uncertainty of tracer, respectively in gas bomb
Compound concentration is 7 × 10-8mg/m31,1,1,2- HFC-134as calibrating gas and concentration be 7 × 10-8mg/m3SF6Standard Gases
Body, after standing 24h to the 36h times, determines 11 tracer concentrations on gas chromatograph respectively, calculates and evaluate relative standard
Deviation, the confidence level of its analysis is illustrated with this；1,1,1,2- HFC-134as and traditional gas tracer SF6Uncertainty
Comparison diagram as shown in Figure 2, in Fig. 2 HFC-134a for HFA 134a abbreviation；Figure it is seen that tetrafluoro second
Alkane relative standard deviation (RSD) is 1.09%, SF6Relative standard deviation is that 1.88%, RSD illustrates its analysis method less than 2%
It is feasible, and the method for testing uncertainty of HFA 134a is better than SF6Method of testing uncertainty.
4. the HFA 134a is tested as the minimum detectability of tracer, is added in gas cylinder respectively
1mL concentration is 3mg/m31,1,1,2- HFC-134as and 3mg/m3SF6Calibrating gas, and with high pure nitrogen with 10 times for step
Length carries out stepwise dilution, by the gaseous sample of each stepwise dilution through gas chromatographic detection, when signal value is less than 3 times of baseline noises
Concentration, the method detection limit of as detected gas tracer；By experiment, the detection for finally measuring HFC-134a is limited to 3
×10-12mg/m3, and under same experiment condition, SF6Minimum detectability be 3 × 10-11mg/m3, illustrate 1,1,1,2- tetrafluoro
The detection limit of ethane is better than SF6Detection limit.
5. the HFA 134a is tested as the determination of recovery rates of tracer, prepares dense in nitrogen cylinder respectively
Spend is 7 × 10-8mg/m31,1,1,2- HFC-134as calibrating gas and concentration be 7 × 10-8mg/m3SF6Calibrating gas；Through
Vibration stands after mixing, and then by its concentration of gas chromatographic detection, actual concentrations and theoretical concentration ratio are final returning
Yield；By 5 experiments, it is 92.23% finally to measure the lowest rate of return of HFA 134a, and highest recovery is
103.32%, average recovery rate is 97.43%, SF6Lowest rate of return be 90.10%, highest recovery is 102.83%, put down
The equal rate of recovery is 96.15%；Determination of recovery rates experimental result all meets 90% to 130% claimed range, and 1,1,1,2- tetra-
The average recovery rate of fluoroethane is better than SF6Average recovery rate.
6. the HFA 134a is tested as the adsorptivity of tracer, coal is ground, with 80 mesh to 100 purposes
Screen cloth is screened, and then carries out ash disposal, and the coal particles after ash disposal are weighed into 9g is filled into internal diameter for 0.6cm, and length is 3m
Stainless steel steel column in, coal particles volume mass is about 0.1g/cm in steel column3；The compound concentration in gas cylinder respectively
It is 5 × 10-9mg/m31,1,1,2- HFC-134as gas and concentration be 5 × 10-9mg/m3SF6Gas, by 1,1,1,2- tetra-
Fluoroethane and SF6Slowly it is passed through in stainless steel steel column, and gas is gathered in the port of export, is detected using gas-chromatography, and count
Concentration is calculated, determines its coal to tracing agent adsorbtion performance by change in concentration situation；By experiment, 1,1,1,2- tetra- is finally measured
It is 1.9% that the average adsorption rate of fluoroethane only has the average adsorption rate of 0.7%, SF6, and the adsorption rate of HFC-134a is less than SF6。
Embodiment 2, multicolored gulf colliery uses mining adjacent phases continuous stoping method, in order to determine air leakage source
With remittance of leaking out, tunnel around B1, B2 and B3 work face goaf and fire dam pressure distribution are determined.By determining,
Purpose and point of release according to investigating should be at the principle of the air leakage source of goaf energy position higher, near selection B2 working face afterbodys
B1 goafs be SF6Point of release, to investigate the air leakage distribution in adjacent sections goaf；Mouth face end support under selection B3 working faces
Afterbody is HFA 134a point of release, is distributed with goaf air leaking after investigating B3 faces.
In order to investigate goaf leaking out on 4 directions, sampled point is determined by site inspection and measure of resistance result, i.e.,
No. 1 Samples selecting is sampled in B1 return airways are closed by peep hole；No. 2 Samples selectings lead in B2 return airways are closed
Cross peep hole sampling；No. 3 Samples selectings are sampled in B3 Bu Jiang lanes are closed by peep hole；No. 4 Samples selectings are in B3Work
Make face upper corner.On June 14 13:50 in B1Mouth face end support frame afterbody release SF under working face6；On June 14 14:30 in B3Work
Make release 1,1,1,2- HFC-134as of being drilled on face；On sampling analysis time from June 14 13:On 50 to June 19 11:30, No. 1 are adopted
On sampling point June 15 5:SF is analyzed in 50 gas sample6, 16h is lasted, a length of 320m of this glide path, therefore from SF6Point of release is to No. 1
Maximum between sampled point leaks out wind speed for 0.4m/min；No. 1 sampled point from release SF6To 18 days 10 June:50,93h is lasted,
Without SF in gas sample6, illustrate SF6Do not exist the wind speed that leaks out or leak out between point of release and No. 1 sampled point less than inflammable wind speed；No. 2 are adopted
On sampling point June 18 6:00 first time analyzed SF6, SF is analyzed for the first time with No. 1 sampled point6Difference 10h 50min；No. 2 sampled points
From release 1,1,1,2- HFC-134as to 18 days 11 June:00,93h 30min are lasted, HFC-134a is had no in gas sample, illustrate four
Do not exist the wind speed that leaks out or leak out between fluoroethane point of release and No. 2 sampled points less than inflammable wind speed；No. 3, No. 4 sampled points are from release
SF697h, SF is not analyzed in all gas samples afterwards6Gas, illustrates SF6Do not exist between point of release and No. 3, No. 4 sampled points
The wind speed that leaks out or leak out is less than inflammable wind speed.
No. 3 14 days 16 sampled point June：10 first times analyzed HFA 134a, lasted 100min, glide path
250m long, therefore it is 2.5m/min to the maximum to the wind speed that leaks out No. 3 sampled points from HFA 134a point of release；No. 4
On sampled point June 14 18：10 first times analyzed HFA 134a, lasted 220min, this glide path 660m long, can
Think to be about 3.3m/min to the wind speed that leaked out No. 4 sampled points from 1,1,1,2- HFC-134as point of release；No. 4 samplings simultaneously
O'clock from 18:HFA 134a concentration gradually increased after 30, to 15 days 7 June:20 gradually reduced, to 16 days 9 June:50
It is not wholly absent also；Illustrate B1Working face and No. 4 leaking out for sampled point are by B1And B3Between coal column crack produce；
Fig. 3 is the concentration standard curve of HFA 134a, for determining the tracer concentration for detecting.
Spike operation is carried out to colliery by dual tracer, wind speed in coal seam can be measured, it is determined that region of leaking out,
And benefit slurry can be carried out to the passage that leaks out, and gas ingredients and its change in concentration are determined, spontaneous combustion forecast is carried out, to take in time
Measure；Double search gas technologies are successfully applied to A mining areas first, it was demonstrated that leak out and be in double tracer technique detection underground goafs
Feasible, the application of double search gas technologies greatly reduces sampling work amount, saves the time, takes full advantage of experiment and sets
Standby and facility, improves operating efficiency.
Embodiment 3, double search gas that the experiment of Changji Hui Autonomous Prefecture, Xinjiang Dahuangshan Coal Mine underground site is used are respectively SF6With 1,1,1,
2- HFC-134a gases, by drilling in the closed inner release SF of -440m first passages6Gas and released at -440m second channels
Put HFA 134a gas, -360m parking lots it is closed, -320m parking lots are closed, -300m parking lots are closed, -250m the 3rd
Gas sample is gathered at the closed grade 4 of passage, each sampled point is not detected by SF6Gas；Other sampled points are examined in addition to -320m parking lots
Measure 1,1,1,2- HFC-134a gases；It is the main air leakage source in the coal mine gob that -440m first passages are closed；The colliery is mined out
Passage mainly leak out for -250m third channels in area；In addition, -360m parking lots it is closed, -300m parking lots are closed, -250m threeways
HFA 134a gas is all detected at road etc. 3, illustrates that HFA 134a gas passes through at -320m parking lots,
May be very fast due to flow velocity, miss the sampling time；It is not detected by SF6The reason for gas is probably：Due to goaf air leaking amount
Greatly, wind speed is very fast, there is SF6Gas sample is not collected in the time period of gas.
By monitoring result, have to the coal mine gob field conduct fire-fighting measure：Whitewashing, slip casting closure air leakage source and
Leak out passage, based on closing of whitewashing.Maintenance tunnel, lays track, recovers transport, and the remittance fire dam that leaks out, tunnel are sprayed
Pressed before slurry, fire dam, reduce fire dam air-out；Fire dam can be set up, then carries out grouting and reinforcing；Other points are the remittance needs that leak out
Progressively maintenance tunnel, slip casting or sets up fire dam grouting and reinforcing leak stopping again；Then mine ventilation, water supply, grouting, note nitrogen etc. are carried out
System call interception, is transformed with reference to mine technology.
After carrying out laddering gas pumping pattern, due to the guarantee for having the extraction time, the coal-bed gas in extraction region
Content is fallen below in safe range, and gas bearing capacity and outburst amount are substantially reduced, and reduces face with air quantity, become local protrusion-dispelling into
Region extinction, eliminates gas hidden danger, improves the mine safety degree of reliability；The relatively low detection limit of HFA 134a,
The features such as sensitivity is high, more traditional tracer SF6Input amount is greatly reduced, cost is greatly reduced, benefit is improve；Can lead to
Cross dual tracer 1,1,1,2- HFC-134as and SF6Cooperation, important application has been obtained in colliery spike construction, real to instructing
Remedial measure is applied there is provided data supporting.
Embodiment 4, Turfan Qi Quanhu collieries are low-permeable high gas layer, gas of being constructed in the A scope of operations of underground
Extraction trial boring, first need to be without joint when coal bed gas drainage radius is determined using HFA 134a trace method
Arrangement one is used to note drilling and a gas-removing extraction testing bore holes of HFA 134a gas in development coal seam, then
HFA 134a gas is noted in injecting hole, then whether is entered by the HFA 134a gas observed in injecting hole
Enter in extraction drilling to determine gas drainage under suction radius, so that it is determined that the cloth pitch of holes of extraction drilling.
During measure, No. 1 extraction testing bore holes are connected with gas drainage pipe first；Injecting hole valve is opened, using 1,
HFA 134a gas is injected injecting hole by 1,1,2- HFC-134a gas injection device, treats 1,1,1,2- tetrafluoro in injecting hole
Ethane gas concentration is 5 × 10-8mg/m3, when aperture pressure reaches 13kPa, open No. 1 extraction ports valve door and start to draw out methane, and
By negative pressure of suction control in 10kPa to 15kPa；Needed during extraction daily in 11 points of detection gas that once institute's extraction goes out
The concentration of contained HFA 134a, and make a record.
No. 1 extraction ports valve door is closed, valve is opened after No. 2 extraction holes are connected with releasing pipe, start to enter No. 2 extraction holes
Row extraction, concentration is gradually reduced, and after after concentration stabilization, No. 2 extraction ports valves is closed, after No. 3 extraction holes are connected with releasing pipe
Valve is opened, starts to carry out extraction to No. 3 extraction holes, concentration is gradually reduced, after after concentration stabilization, close No. 3 extraction ports valves,
Valve is opened after No. 4 extraction holes are connected with releasing pipe, starts to carry out extraction to No. 4 extraction holes, concentration is gradually reduced, to No. 4
Be can't detect during door, illustrate that this hole is not influenceed in extraction by injecting hole.
Gas drainage under suction radius can be identified as No. 3 extraction holes and arrive the distance between injecting hole, i.e. 4m to 5m with No. 4 extraction holes；
It is 4m or 5m that the gas drainage under suction radius determined using HFA 134a gas tracer method can be fixed tentatively, in order to determine essence
True drainage radius, scene is also needed to drainage radius as the gas drainage under suction effect that the extraction of 3m and 4m drills is analyzed.
Found by the A working faces live gas pumping contrast test of nearly 3 months, when radius is 4m, average extraction
Rate is 35%；When radius is 5m, average extraction rate is 28%.Therefore, Turfan Qi Quanhu applies in colliery 1,1,1,2- tetrafluoro
The gas drainage under suction radius that ethane gas trace method is determined is defined as 4m；Determined by 1,1,1,2- HFC-134as gas tracer method
Gas drainage results are carried on the original basis with relative gas pressure measurement method gas drainage results comparative analysis, the gas density in releasing pipe
High by 8%, negative pressure declines about 42%, and gas pumping rate brings up to more than original twice, and the gas density in return is few
In half before, and there is no invar this problem again and cause working face circut breaking；1,1,1,2- HFC-134as extraction half
On extraction rate influence situation comparison diagram as shown in Figure 4, when as can be seen from Figure 4 drainage radius are 4m, extraction rate is high in footpath；Using
1,1,1,2- HFC-134a tracers determine that drainage radius method is feasible.
Because the detection limit of HFA 134a is low, detection sensitivity is high, when gas drainage under suction radius is determined
Relative to traditional tracer SF6The input amount of tracer can be reduced, under the same conditions, the dispensing of HFA 134a
Amount only needs traditional tracer SF6/ 10th of injected volume, so as to greatly reduce cost.
In sum, present invention firstly discloses HFA 134a as tracer in coal mine gas should
With；The more traditional tracer SF of 1,1,1,2- HFC-134as6With sensitivity is high, good stability, adsorbance is few etc. in the middle of coal seam
Advantage, especially detection limit is very low, and minimum detectability can reach 3 × 10-12mg/m3, consumption is few, low cost, compared to biography
System tracer SF6There is obvious advantage；HFA 134a environmental protection simultaneously, small to depletion of the ozone layer, the residence time is short,
Can rapidly be degraded in air, preferably can be applied in coal mine gas as tracer.
Above technical characteristic constitutes embodiments of the invention, and it has stronger adaptability and implementation result, can basis
The non-essential technical characteristic of increase and decrease is actually needed to meet the demand of different situations.
Claims (1)
1. application of a kind of 1,1,1,2- HFC-134as as tracer in coal mine gas.
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| CN201710018833.4A CN106706819A (en) | 2017-01-10 | 2017-01-10 | Application of 1,1,1,2-tetrafluoroethane used as tracer in coal mine gas |
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| CN201710018833.4A CN106706819A (en) | 2017-01-10 | 2017-01-10 | Application of 1,1,1,2-tetrafluoroethane used as tracer in coal mine gas |
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Application publication date: 20170524 |