CN102998204A - Device and method for preparing water-containing coal sample and testing adsorption - Google Patents
Device and method for preparing water-containing coal sample and testing adsorption Download PDFInfo
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- CN102998204A CN102998204A CN201210558218XA CN201210558218A CN102998204A CN 102998204 A CN102998204 A CN 102998204A CN 201210558218X A CN201210558218X A CN 201210558218XA CN 201210558218 A CN201210558218 A CN 201210558218A CN 102998204 A CN102998204 A CN 102998204A
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Abstract
The invention discloses a device and a method for preparing a water-containing coal sample and testing adsorption. The device mainly consists of a sample room, a reference room, a control valve, a pressure transmitter, an air injection pump, a data collection card, a collection terminal, a filter and a thermostatic water bath. According to the device and the method for preparing the water-containing coal sample and testing the adsorption, the preparation of the water-containing coal sample can be realized by stimulating a coal bed ground water pressure-bearing environment, and the air adsorbing capacity testing can be carried out, wherein the method comprises the following steps of: carrying out vacuumizing on a system, injecting ground water sample by vacuum suction of the system, ensuring that the coal sample is submerged in the ground water, injecting helium into the system by the air injection pump, and enabling a pore water pressure of the coal sample to reach a ground water pressure; converging superfluous water of the coal sample to the bottom of the sample room under the effect of gravity, and discharging the superfluous water under the effect of an air pressure to finish the preparation of the coal sample; and after carrying out vacuumizing on the system, injecting adsorbed air into the reference room by the air injection pump, controlling classification and injecting the air into the sample room through the valve, after the adsorption is balanced, counting the adsorbing capacity. According to the device and the method for preparing the water-containing coal sample and the testing adsorption, the structure is simple, the operation is convenient, and the application prospect is wide.
Description
Technical field
The present invention relates to a kind of moisture coal sample preparation and adsorption measuring device and method, belong to porous medium physical and chemical adsorption technical field of measurement and test, be particularly useful for simulating the sample preparation and the gas absorption that contain the aqueous water coal sample under the large buried depth geologic condition and measure examination.
Background technology
In the cbm development process, coal is to carry out Reserves Evaluation, rationally carry out one of the basis of coal-bed gas exploitation to the adsorptive power of gas.Studies show that: gas is subjected to the reservoir environmental impact take ADSORPTION STATE as main in the coal, and various gases are in the competitive Adsorption state.Conscientiously simulate the reservoir environment, considering various effect of complicate factors is to estimate coal measures examination to gas absorption key.In the reality, in burying darker coal seam, after underground water entered the coal seam, before the drainage and step-down exploitation, the pressure of aqueous water was larger, and this part water can overcome surface tension and enter in the micro-pore, and gas absorption is exerted an influence.
At present, the many modes by Vapor adsorption or immersion aqueous water of moisture preparation of coal prepare, the form of water has larger difference in the prepared moisture coal sample of this mode and the real coal seam reservoir, experimental result also will depart from reality, not reflect that aqueous water affects gas absorption in the real coal seam.The adsorption instrument that at present test is adopted also only is used for adsorbance mostly to be measured, and does not have the preparation of simulation reservoir characteristics and contains aqueous water coal sample function, and this has caused great trouble to experiment.For the problems referred to above, be necessary to design and a kind ofly can simulate coal seam reservoir characteristics preparation and contain the aqueous water coal sample equipment that the line correlation gas absorption measures of going forward side by side.
Summary of the invention
Technical matters: the objective of the invention is to overcome the deficiency in the prior art, provide the high coal seam reservoir characteristics preparation of can simulating of a kind of simple in structure, easy to operate, Real-time Collection, good stability, measurement efficient and precision to contain the aqueous water coal sample apparatus and method that the line correlation gas absorption measures of going forward side by side.
Technical scheme: moisture coal sample preparation of the present invention and absorption proving installation comprise acquisition terminal, constant temperature water bath, sample chamber, reference chamber, reference pressure chamber transmitter, sample chamber pressure unit, gas injection pump, data collecting card, reference chamber gas outlet, stopple coupon, sample preparation drainpipe, filtrator; Described reference chamber top connects respectively reference pressure chamber transmitter, gas injection pump and reference chamber gas outlet through four-way, and the pipeline that connects the gas injection pump is provided with air intake control valve, and the reference chamber gas outlet is provided with the reference pressure chamber operation valve; Top, described sample chamber connects respectively the bottom of sample chamber pressure unit, stopple coupon and reference chamber through four-way, and stopple coupon is provided with the sampling operation valve, and the pipeline that connects the bottom of reference chamber is provided with the absorption and control valve; The bottom of described sample chamber connects the sample preparation drainpipe, and the sample preparation drainpipe is provided with the sample preparation draining control valve; Described reference pressure chamber transmitter, sample chamber pressure unit are connected with acquisition terminal through data collecting card respectively; Described sample chamber, reference chamber, sample preparation draining control valve, absorption and control valve, reference pressure chamber operation valve, sampling operation valve, air intake control valve place constant temperature water bath.
Described sample chamber, reference chamber are vertically settled, and its bottom is and forms funnelform taper or circle; Bottom, described sample chamber is provided with filtrator with sample preparation drainpipe junction.
Utilize said apparatus to realize containing the method for the preparation of aqueous water coal sample and gas absorption measurement, comprise the steps:
A, coal sample is put into the sample chamber, opens sample preparation draining control valve, absorption and control valve, connect vacuum pump from the sample preparation drainpipe, system is vacuumized processing, when vacuumize finish after, close sample preparation draining control valve, absorption and control valve;
B, open the sampling operation valve and slowly suck sampling of ground water from stopple coupon, during coal sample in volume of water sample floods the sample chamber, close the sampling operation valve, record sucks the volume of water sample of sample chamber;
C, open air intake control valve, absorption and control valve, enter helium by the gas injection infusion, the pressure of helium increases to the groundwater pressure of required simulated formation, leaves standstill a period of time, closes air intake control valve, open the sample preparation draining control valve, unnecessary water sample is pooled to the bottom, sample chamber in the sample chamber under Action of Gravity Field, depresses at gas, discharge the volume of record drainage water by the sample preparation drainpipe;
Behind d, the discharge excessive moisture, close air intake control valve, sample preparation draining control valve, absorption and control valve, connect vacuum pump from the reference chamber gas outlet reference chamber is vacuumized processing, in vacuumizing processing procedure, be interrupted and open the absorption and control valve, to remove the helium in the sample chamber;
E, vacuumize finish after, close absorption and control valve, reference pressure chamber operation valve, finish and contain aqueous water coal sample preparation;
F, inject the adsorbed gas of required measurement in the reference chamber with the gas injection pump, the gaseous tension in the record reference chamber is opened the absorption and control valve, in the sample chamber, inject adsorbed gas, record sample chamber change value of pressure after the pressure equilibrium upon adsorption, carries out the absorption of next stage pressure and measures.
If need further to reduce the coal sample water percentage, open air intake control valve, adopt the gas injection pump, constantly pass into dry helium gas to the sample chamber through reference chamber, make dry helium gas carry sample chamber coal sample steam and discharge from the sample preparation drainpipe;
If need to accelerate the water percentage changing down, open air intake control valve, constantly pass into dry helium gas by the gas injection pump to the sample chamber through reference chamber, dry helium gas coal sample steam in carrying the sample chamber improves the constant temperature water bath temperature from the process that the sample preparation drainpipe is discharged;
When carrying out the mixed gas sorption measurement and need collected specimens chamber gas to carry out component analysis, carry out gas sample by stopple coupon.
Beneficial effect: it is historical that the present invention can simulate coalbed methane reservoir underground water pressure-bearing, preparation reflection reservoir environmental quality contain the aqueous water coal sample, the promoting the circulation of qi body adsorbance of going forward side by side test realizes that sample preparation is integrated with the absorption measuring process, pressure changes employing and automatically detects, and automaticity is high.Its structure and method is simple, and is easy to operate, and purposes is wide, practical, with a wide range of applications.
Description of drawings
Fig. 1 is moisture coal sample preparation of the present invention and adsorption measuring device structural representation.
Among the figure: the 1-sample chamber; The 2-reference chamber; 3-sample preparation draining control valve; 4-absorption and control valve; 5-reference pressure chamber operation valve; The 6-operation valve of taking a sample; 7-reference pressure chamber transmitter; 8-sample chamber pressure unit; The 9-air intake control valve; 10-gas injection pump; The 11-data collecting card; The 12-acquisition terminal; 13-reference chamber gas outlet; The 14-stopple coupon; 15-sample preparation drainpipe; The 16-filtrator; The 17-constant temperature water bath.
Embodiment
Below in conjunction with accompanying drawing one embodiment of the present of invention are further described:
Moisture coal sample preparation of the present invention mainly is comprised of sample chamber 1, reference chamber 2, sample preparation draining control valve 3, absorption and control valve 4, reference pressure chamber variable valve 5, sampling operation valve 6, reference pressure chamber transmitter 7, sample chamber pressure unit 8, air intake control valve 9, gas injection pump 10, data collecting card 11, acquisition terminal 12, reference chamber gas outlet 13, stopple coupon 14, sample preparation drainpipe 15, filtrator 16, constant temperature water bath 17 with adsorption measuring device.Described sample chamber 1, reference chamber 2 are vertically settled, and its bottom is taper or circle, forms funnel-form; 1 bottom, described sample chamber and sample preparation drainpipe junction are provided with filtrator 16.Reference chamber 2 tops connect respectively gas injection pump 10, reference pressure chamber transmitter 7, reference chamber gas outlet 13 through four-way, and the pipeline that connects gas injection pump 10 is provided with air intake control valve 9, and reference chamber gas outlet 13 is provided with reference pressure chamber operation valve 5; 1 top, described sample chamber connects respectively the bottom of sample chamber pressure unit 8, stopple coupon 14 and reference chamber 2 through four-way, and stopple coupon 14 is provided with sampling operation valve 6, and the pipeline that connects the bottom of reference chamber 2 is provided with absorption and control valve 4; The bottom of described sample chamber 1 connects sample preparation drainpipe 15, connecting interface place placement filter device 16, and sample preparation drainpipe 15 is provided with sample preparation draining control valve 3; Described reference pressure chamber transmitter 7, sample chamber pressure unit 8 are connected with acquisition terminal 12 through data collecting card 11 respectively; Described sample chamber 1, reference chamber 2, sample preparation draining control valve 3, absorption and control valve 4, reference pressure chamber operation valve 5, sampling operation valve 6, air intake control valve 9 place constant temperature water bath 17.
Moisture coal sample preparation of the present invention and absorption method of testing:
Moisture coal sample preparation: coal sample is put into sample chamber 1, open sample preparation draining control valve 3, absorption and control valve 4, connect vacuum pump from sample preparation drainpipe 15, system is vacuumized processing, when vacuumize finish after, close sample preparation draining control valve 3, absorption and control valve 4; Open sampling operation valve 6 and slowly suck sampling of ground waters from stopple coupon 14, during coal sample when volume of water sample floods sample chamber 1 in, close sampling operation valve 6, the volume of water sample of record suction sample chamber 1; Open air intake control valve 9, absorption and control valve 4, inject helium by gas injection pump 10, the pressure of helium increases to the groundwater pressure of required simulated formation, leave standstill 24 hours after, close air intake control valve 9; Open sample preparation draining control valve 3, unnecessary water sample is pooled to 1 bottom, sample chamber in the sample chamber 1 under Action of Gravity Field, depresses at gas, discharges the volume of record drainage water by sample preparation drainpipe 15; After discharging excessive moisture, close air intake control valve 9, sample preparation draining control valve 3, absorption and control valve 4, connect vacuum pump from reference chamber gas outlet 13 reference chamber 2 is carried out application of vacuum, in vacuum, open absorption and control valve 4 every 30 minutes and continue 5 minutes, continue 10 times, remove the helium in the sample chamber 1.Vacuumize finish after, close absorption and control valve 4, reference pressure chamber operation valve 5, finish and contain aqueous water coal sample preparation;
The unnecessary water sample of coal sample is pooled to 1 bottom, sample chamber and discharges fully by sample preparation drainpipe 15 under Action of Gravity Field, if need further to reduce the coal sample water percentage, open air intake control valve 9, adopt gas injection pump 10,1 constantly pass into dry helium gas through reference chamber 2 to the sample chamber, make dry helium gas carry sample chamber 1 coal sample steam and discharge from sample preparation drainpipe 15, pass into and improve constant temperature water bath 17 temperature in the helium process.
Adsorbance is measured: inject the adsorbed gas of required measurement, record reference chamber gaseous tension in the reference chamber 2 with gas injection pump 10.Open absorption and control valve 4, in sample chamber 1, inject adsorbed gas, record sample chamber change value of pressure, wait upon the adsorptive pressure balance after, carry out the absorption of next stage pressure and measure.When carrying out the mixed gas sorption measurement and needing collected specimens chamber gas to carry out component analysis, carry out gas sample by stopple coupon 14.
Claims (7)
1. a moisture coal sample prepares and the absorption proving installation, comprise acquisition terminal (12), constant temperature water bath (17), it is characterized in that: also comprise sample chamber (1), reference chamber (2), reference pressure chamber transmitter (7), sample chamber pressure unit (8), gas injection pump (10), data collecting card (11), reference chamber gas outlet (13), stopple coupon (14), sample preparation drainpipe (15), filtrator (16); Described reference chamber (2) top connects respectively reference pressure chamber transmitter (7), gas injection pump (10) and reference chamber gas outlet (13) through four-way, the pipeline that connects gas injection pump (10) is provided with air intake control valve (9), and reference chamber gas outlet (13) is provided with reference pressure chamber operation valve (5); Top, described sample chamber (1) connects respectively the bottom of sample chamber pressure unit (8), stopple coupon (14) and reference chamber (2) through four-way, stopple coupon (14) is provided with sampling operation valve (6), and the pipeline that connects the bottom of reference chamber (2) is provided with absorption and control valve (4); The bottom of described sample chamber (1) connects sample preparation drainpipe (15), and sample preparation drainpipe (15) is provided with sample preparation draining control valve (3); Described reference pressure chamber transmitter (7), sample chamber pressure unit (8) are connected with acquisition terminal (12) through data collecting card (11) respectively; Described sample chamber (1), reference chamber (2), sample preparation draining control valve (3), absorption and control valve (4), reference pressure chamber operation valve (5), sampling operation valve (6), air intake control valve (9) place constant temperature water bath (17).
2. moisture coal sample preparation according to claim 1 and absorption proving installation, it is characterized in that: described sample chamber (1), reference chamber (2) are vertically settled, and its bottom is and forms funnelform taper or circle.
3. moisture coal sample preparation according to claim 1 and absorption proving installation, it is characterized in that: described sample chamber (1) bottom is provided with filtrator (16) with sample preparation drainpipe junction.
4. utilize claim 1,2 or 3 described devices to realize the method that moisture coal sample preparation and absorption are tested, it is characterized in that, comprise the steps:
A, coal sample is put into sample chamber (1), open sample preparation draining control valve (3), absorption and control valve (4), connect vacuum pump from sample preparation drainpipe (15), system is vacuumized processing, when vacuumize finish after, close sample preparation draining control valve (3), absorption and control valve (4);
B, open sampling operation valve (6) and slowly suck sampling of ground water from stopple coupon (14), during coal sample when volume of water sample floods sample chamber (1) in, close sampling operation valve (6), the volume of water sample of record suction sample chamber (1);
C, open air intake control valve (9), absorption and control valve (4), inject helium by gas injection pump (10), the pressure of helium increases to the groundwater pressure of required simulated formation, leaves standstill a period of time, closes air intake control valve (9), open sample preparation draining control valve (3), unnecessary water sample is pooled to bottom, sample chamber (1) in the sample chamber (1) under Action of Gravity Field, depresses at gas, discharge the volume of record drainage water by sample preparation drainpipe (15);
Behind d, the discharge excessive moisture, close air intake control valve (9), sample preparation draining control valve (3), absorption and control valve (4), connect vacuum pump from reference chamber gas outlet (13) reference chamber (2) is vacuumized processing, in vacuumizing processing procedure, be interrupted and open absorption and control valve (4), to remove the helium in the sample chamber (1);
E, vacuumize finish after, close absorption and control valve (4), reference pressure chamber operation valve (5), finish and contain aqueous water coal sample preparation;
F, usefulness gas injection pump (10) are to the middle adsorbed gas of injecting required measurement of reference chamber (2), gaseous tension in the record reference chamber (2), open absorption and control valve (4), inject adsorbed gas in (1) to the sample chamber, record sample chamber (2) change value of pressure, after the pressure equilibrium upon adsorption, carry out the absorption of next stage pressure and measure.
5. moisture coal sample preparation according to claim 4 and the method for adsorbing test, it is characterized in that: if needs further reduce the coal sample water percentage, open air intake control valve (9), adopt gas injection pump (10), (1) constantly passes into dry helium gas to the sample chamber through reference chamber (2), makes dry helium gas carry sample chamber (1) coal sample steam and discharges from sample preparation drainpipe (15).
6. moisture coal sample preparation according to claim 4 and the method for adsorbing test, it is characterized in that: if need to accelerate the water percentage changing down, open air intake control valve (9), (1) constantly passes into dry helium gas to the sample chamber through reference chamber (2) by gas injection pump (10), and dry helium gas coal sample steam in carrying sample chamber (1) improves constant temperature water bath (17) temperature from the process that sample preparation drainpipe (15) is discharged.
7. the method for moisture coal sample preparation according to claim 4 and absorption test is characterized in that: when carrying out the mixed gas sorption measurement and need collected specimens chamber gas to carry out component analysis, carry out gas sample by stopple coupon (14).
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Cited By (8)
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CN103245539A (en) * | 2013-04-22 | 2013-08-14 | 河南理工大学 | Manufacturing method of coal samples with different water contents |
CN103604663A (en) * | 2013-10-31 | 2014-02-26 | 中国水利水电建设工程咨询西北有限公司 | Sampling and preserving device used for water quality monitoring samples |
CN103994912A (en) * | 2014-05-11 | 2014-08-20 | 中国矿业大学 | Immersion method capable of maintaining structural integrity of coal sample |
CN104697838A (en) * | 2015-03-27 | 2015-06-10 | 河南理工大学 | Coal sample water injection device for simulating high-pressure water injection at coal mine site in laboratory |
CN104990833A (en) * | 2015-04-17 | 2015-10-21 | 南京市产品质量监督检验院 | Gas absorbing volume detector and detecting method |
CN105021493A (en) * | 2015-07-13 | 2015-11-04 | 中国石油大学(华东) | Absorption-desorption method of multicomponent gases and device thereof |
CN106198296A (en) * | 2015-06-01 | 2016-12-07 | 中国人民解放军63971部队 | A kind of DMMP concentration determination method |
CN113019080A (en) * | 2019-12-24 | 2021-06-25 | 中核四0四有限公司 | Helium protective gas purification device and method |
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Cited By (12)
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CN103245539A (en) * | 2013-04-22 | 2013-08-14 | 河南理工大学 | Manufacturing method of coal samples with different water contents |
CN103245539B (en) * | 2013-04-22 | 2015-04-22 | 河南理工大学 | Manufacturing method of coal samples with different water contents |
CN103604663A (en) * | 2013-10-31 | 2014-02-26 | 中国水利水电建设工程咨询西北有限公司 | Sampling and preserving device used for water quality monitoring samples |
CN103604663B (en) * | 2013-10-31 | 2016-01-20 | 中国水利水电建设工程咨询西北有限公司 | A kind of water quality monitoring sample save set |
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CN104697838B (en) * | 2015-03-27 | 2017-09-05 | 河南理工大学 | A kind of coal sample water filling device of laboratory simulation colliery scene high pressure water injection |
CN104990833A (en) * | 2015-04-17 | 2015-10-21 | 南京市产品质量监督检验院 | Gas absorbing volume detector and detecting method |
CN106198296A (en) * | 2015-06-01 | 2016-12-07 | 中国人民解放军63971部队 | A kind of DMMP concentration determination method |
CN105021493A (en) * | 2015-07-13 | 2015-11-04 | 中国石油大学(华东) | Absorption-desorption method of multicomponent gases and device thereof |
CN105021493B (en) * | 2015-07-13 | 2017-11-28 | 中国石油大学(华东) | A kind of absorption analysis method and device of multicomponent gas |
CN113019080A (en) * | 2019-12-24 | 2021-06-25 | 中核四0四有限公司 | Helium protective gas purification device and method |
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