CN103698186B - Transformation controllable gas displacement reaction device and the application in the gassiness preparation of soil sample thereof - Google Patents

Transformation controllable gas displacement reaction device and the application in the gassiness preparation of soil sample thereof Download PDF

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CN103698186B
CN103698186B CN201310752757.1A CN201310752757A CN103698186B CN 103698186 B CN103698186 B CN 103698186B CN 201310752757 A CN201310752757 A CN 201310752757A CN 103698186 B CN103698186 B CN 103698186B
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reactor
graduated cylinder
gas
gland bonnet
pressure
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CN103698186A (en
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王勇
孔令伟
杨爱武
王艳丽
许鹏程
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Wuhan Institute of Rock and Soil Mechanics of CAS
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Wuhan Institute of Rock and Soil Mechanics of CAS
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Abstract

The invention belongs to manual simulation's sample preparation experimental technique field of Geotechnical Engineering seabed gas-containing sediment, specifically disclose a kind of transformation controllable gas displacement reaction device and the application in the gassiness preparation of soil sample thereof.This device comprises the reactor and graduated cylinder that are fixed on same base upper surface, by regulating the pressure in reactor and graduated cylinder, realizes the accurate measurement of gas displacement reaction under different pressures and gas quantum of output; Under can setting up constant temperature, the quantitative relationship in different pressures environment between the quality of gas adsorbability solid particle and its gas displaced, based on this relation, realizes the artificial fixing quantity of the gassiness preparation of soil sample.In preparation soil sample, the crystal structure special by zeolite and strongly hydrophilic, and zeolite proportion is close with soil particle proportion, by the zeolite granular of the saturated methane gas of absorption and soil particle Homogeneous phase mixing, then add water, displace the methane gas adsorbed in zeolite granular with water, thus form the bubbles soil body, prepared gassiness soil sample is even.

Description

Transformation controllable gas displacement reaction device and the application in the gassiness preparation of soil sample thereof
Technical field
The present invention relates to manual simulation's sample preparation experimental technique field of Geotechnical Engineering seabed gas-containing sediment, be specifically related to a kind of transformation controllable gas displacement reaction device and the application in the gassiness preparation of soil sample thereof.
Background technology
Submarine shallow gas is often referred to the gas assembled in sediment within 1000m below sea bottom surface.The component of shallow gas mainly comprises methane, carbon dioxide, sulfuretted hydrogen, ethane etc., wherein general the highest with methane content, is generally distributed in the stratum, marine site of the waters such as lake, river valley, bay, delta and oily resource relative abundance.Gas mainly stems from biogenetic gas that organic matter decomposition formed and Deep Oil-gas, earth mantle and magmation institute migrate through top the gas be closed in superficial part sedimentary deposit postpartum.Gas is often composed with occurrence patterns such as free bubble, dissolving or water compounds and is stored in sediment, is often called gas hydrate by composing the gas-containing sediment deposited with hydrate, and is called gassiness soil by composing the gas-containing sediment deposited with free gas, solution gas form.
The gas be rich in gassiness soil can be used as the energy and is used, but because cause engineering proterties to worsen containing gas in soil, can bring disaster to engineering.As often in: seabed gassiness soil cause seashore landslide, the disaster accident such as liquefaction of soil mass, yielding of foundation, oil gas blowout, platform topple, hole collapse, line break, constituting a serious threat to the engineering constructions such as gas and oil in sea and exploitation, drilling platform, port and pier, tunnel over strait, submarine transport oil pipeline and communication cable and inshore infrastructure, is the important safety hidden danger in oceanographic engineering.
Gassiness soil is considered to the product of soil particle, pore water, gas, pressure, temperature and superstratum perfection balance, once balance is broken, its engineering proterties will be caused to change rapidly.Although people have recognized that the harmfulness problem of seabed gassiness soil, but the scientific research carried out is very limited, especially lack the research to its soil mechanics characteristic, it is large that main difficulty comes from air in soil body pressure, and be easy to loss, be difficult to obtain on-the-spot original state gassiness soil soil sample.Even if adopt special equipment can obtain pressurize undisturbed soil sample, be still subject to too high to shop experiment environmental requirement, to be difficult to the problems such as secondary processing, sample be uneven puzzlement, impel indoors artificial analogue technique to become the basic technology of such soil of research.
What first manual simulation needed to solve is exactly the sample preparation problem of gassiness soil.At present, have and adopt anaerobic fermentation microorganism to mix with soil particle, in adapt circumstance, utilize fermentable to produce methane gas, simulate the natural forming process of gassiness soil, and then make the method for gassiness soil sample.But this method is time-consuming, effort, the more important thing is that the gassiness air in soil scale of construction cannot realize artificial fixing quantity, made sample is uneven, and sample room does not possess repeatability, specific model investigation can only be used for, and cannot use for general indoor triaxial test.Also the preparation method adopting unsaturated soil is had, utilize air or nitrogen progressively in displacement saturated soil the method for moisture to prepare the method for gassiness soil sample, but the method can only be prepared saturation degree and be less than 85%, the consecutive soil sample of air in soil, and gas exists with free bubble form in the seabed gassiness warp of reality, saturation degree is generally all greater than 85%, therefore the method also effectively cannot realize manual simulation's preparation of seabed gassiness soil sample.
Summary of the invention
For the deficiencies in the prior art, one object of the present invention there are provided a kind of transformation controllable gas displacement reaction device, utilize this device can realize the fixing quantity of air in soil body burden under different pressures environment, and then prepare the gassiness soil sample meeting requirement of experiment.This goal of the invention is achieved through the following technical solutions:
A kind of transformation controllable gas displacement reaction device, comprise reactor, graduated cylinder and base, described reactor and graduated cylinder are fixed on base upper surface;
For ease of the level change of external observation reactor inside, the sidewall of described reactor is provided with vertical view window, and view window is transparent material, can select transparent resistance to laminated glass, be assembled into one with reaction kettle body, and keeps leakproofness and the resistance to pressure of whole reactor.
Described reactor and graduated cylinder upper end open, be stamped reactor gland bonnet and graduated cylinder gland bonnet respectively, and further, reactor and reactor gland bonnet, graduated cylinder and graduated cylinder gland bonnet are all threaded connection, and ensures the airtight of reactor and graduated cylinder;
Described reactor is prepared from by high pressure resistant material, and it is withstand voltage, and the limit is not less than 5MPa, and the volume of reactor can be determined as required;
The outside surface of described reactor gland bonnet is plane, and inside surface is the taper shape of indent, in reactor gland bonnet, form an indent cone-shaped space, makes reactor gland bonnet be the cover body structure of the thick intermediate thin in edge;
The conical top perforate of described reactor gland bonnet inside surface indent, tapping establishes reactor porting, the pipeline of described reactor porting is provided with reactor tensimeter, the opening part of described reactor porting is provided with reactor intake and exhaust valve, reactor intake and exhaust valve is discharged for controlling or is filled with reaction gas reactor, and reactor tensimeter is then for measuring the pressure in reactor;
Described reactor gland bonnet is also provided with a water inlet and two freeing port;
Described water inlet is arranged at the side of reactor gland bonnet, described water inlet is opened flat hole and is through to reactor gland bonnet inside surface, the aperture place of inside surface is provided with water inlet pipe, water inlet pipe passes from the indent cone-shaped space in reactor gland bonnet and puts in reactor, open the height of flat hole lower than the conical vertex of a cone of indent, like this reactor inside is communicated with outside water inlet system; The pipeline of the outer water inlet of reactor gland bonnet is provided with water inlet valve, and water inlet valve is for cutting off contacting of outside water inlet system and reactor inside, and the withstand voltage limit identical reaction kettle of the water inlet pipe in described reactor, is also not less than 5MPa;
Described two freeing port are respectively the first row mouth of a river and the second row mouth of a river;
The described second row mouth of a river is arranged at the opposite side of reactor gland bonnet, relative with described water inlet, described second row mouth of a river place opens flat hole and is through to reactor gland bonnet inside surface, the highly same water inlet of perforate, the aperture place of inside surface is provided with drainage pipe, described drainage pipe stretches to 3 ~ 5cm place, distance reactor bottom surface in reactor, drainage pipe is made up of filtering head and pressure pipe, filtering head is arranged at the lower end of pressure pipe, filtering head is for filtering the solid particulate matter in reactor, guarantee the solid particulate matter can not taken away in the liquid of discharging in reactor, error is caused to test, the withstand voltage limit identical reaction kettle of described pressure pipe, also 5MPa is not less than,
One end of the external withstand voltage drainage connecting pipe in aperture, the second row mouth of a river of reactor gland bonnet outside, the other end of withstand voltage drainage connecting pipe extends in graduated cylinder through graduated cylinder gland bonnet, and described withstand voltage drainage connecting pipe is provided with the second valve;
The described first row mouth of a river is arranged on the sidewall of reactor gland bonnet, the described first row mouth of a river is between water inlet and the second row mouth of a river, described first row mouth of a river place opens flat hole, perforate height flushes with the conical vertex of a cone of the indent in reactor gland bonnet, flat hole is through to the vertex of a cone of reactor gland bonnet inside surface, the pipeline at the first row mouth of a river outside reactor gland bonnet is provided with the first valve, for cutting off the passage of the outside overflow of liquid in reactor, the object of described reactor gland bonnet structure like this is that liquid is input into after in airtight reactor through water inlet, thoroughly can drain all gas in still, guarantee that reactor inner space is all full of by liquid, and not residual gas.
Due to described graduated cylinder being stamped graduated cylinder gland bonnet, therefore different from general uncovered graduated cylinder, be sealing graduated cylinder container, graduated cylinder adopts withstand voltage transparent material to make cylindrical shape, barrel wall has worn lattice scale for metered volume, and the withstand voltage limit is mated with reactor, is not less than 5MPa;
Described graduated cylinder gland bonnet also offers a hole, this hole is connected with pipeline, and one end of pipeline puts in graduated cylinder; The other end, outside graduated cylinder, is graduated cylinder porting; Pipeline is provided with graduated cylinder tensimeter and graduated cylinder intake and exhaust valve successively along discharge directions, and graduated cylinder tensimeter is for the amount of measurement cylinder pressure.
The entirety of transformation controllable gas displacement reaction device of the present invention and the size of each building block can require to arrange flexibly according to test accuracy, and the precision of cylinder scale can lattice as required.
The rain glass that described two tensimeters (reactor tensimeter and graduated cylinder tensimeter) can select range suitable according to the pressure limit of testing requirements, mechanical type, electric measuring type etc., without other special requirement.
In described transformation controllable gas displacement reaction device, each pipeline/road all needs to meet the extreme pressure requirement consistent with reactor except voltage endurance capability, is namely all not less than beyond 5MPa, and the bore in each pipeline/road is unsuitable excessive, should select
Valve on each pipeline/road, without particular/special requirement, guarantees impermeability with the match specifications in pipeline/road.
Another object of the present invention there are provided a kind of described application of transformation controllable gas displacement reaction device in the gassiness preparation of soil sample, and the technical scheme of this application is as follows:
(1) zeolite granular of selected particle diameter (mate with the soil sample grain diameter of step (3), the particle diameter of zeolite granular is close to the mean grain size of soil particle) to be inserted in baking oven 105 DEG C to carry out drying and dewater, then put into dry cylinder and cool.Under constant indoor temperature condition, take the zeolite granular of the drying cooling of certain mass, insert in reactor and vacuumized by reactor porting, get rid of the air adsorbed in reactor and in zeolite granular, it is saturated that the methane gas then passing into test predetermined pressure by the first row mouth of a river in reactor carries out absorption.Saturated complete after, be rapidly in reactor by water inlet and pass into degassed water until be all full of by water in still, not residual gas.After being filled with the air of test predetermined pressure in graduated cylinder, open the second valve between graduated cylinder and reactor, water in reactor displaces the methane gas adsorbed in zeolite granular, gas converges gradually at reactor top conical shape top, and the water in reactor is under atmospheric pressure effect, to flow in graduated cylinder until test stops (liquid level no longer changes) by drainage pipe, the volume flowing into water in graduated cylinder is the methane gas scale of construction that the zeolite granular of this certain mass displaces under this test pressure.
(2) carry out the gas displacement reaction of different quality zeolite granular under uniform pressure condition according to step (1), the quantitative relationship between zeolite granular quality and gas quantum of output under same pressure environment can be set up out; Carry out the gas displacement reaction of zeolite granular under different pressures condition of equal in quality again, the quantitative relationship between pressure and gas quantum of output can be set up out.Thus, undertaken under test can set up constant temperature by described transformation controllable gas displacement reaction device, pressure, quantitative relationship between zeolite granular quality and gas quantum of output.According to wishing to get in saturation degree gassiness soil contained gas flow, this saturation degree gassiness soil of preparation can be gone out should mix the quality of zeolite granular and required dry ground quality by inverse according to above-mentioned quantitative relationship.
(3) zeolite granular cooled by the drying determining quality in (2) is weighed, insert closed container to vacuumize, at least 24h is preserved under-100kPa pressure, and in backward closed container, be filled with the methane gas of predetermined pressure, deposit at least 24h saturated to methane adsorption, rapid taking-up zeolite granular, insert in the lump in airtight sample preparation device with load weighted dry ground in advance and mix, more than operate 2-5min to complete (from taking-up zeolite granular to mixing), and be set to the remoulded sample of default dry density, this process need keep the pressure in airtight sample preparation device to be that constant specified pressure (has nothing to do with preset pressure above, here can freely specify), the pressure reduction keeping being not more than 5kPa is by degassed water from bottom to top submergence soil sample gradually bottom airtight sample preparation device, air in displacement soil mesoporosity is with saturated soil sample.Soil mesolite particle meets the rearmounted methane gas that swaps out of water, thus is prepared into and can be used for predetermined saturation needed for indoor triaxial test and bubble distribution uniform gassiness soil soil sample.
What deserves to be explained is, because gas temperature influence is remarkable, the preparation process of above-mentioned gassiness soil must be carried out under constant temperature, the reliability of guarantee preparation method and controllability.
The advantage of apparatus of the present invention is that testing equipment is simple, operating process is easy to grasp; Can by regulating the pressure in reactor and graduated cylinder, realize the accurate measurement of gas displacement reaction under different pressures environment and gas quantum of output; Under can constant temperature being set up, in different pressures environment the quality of gas adsorbability solid particle and its displace quantitative relationship between gas yield, based on this relation, thus realize the artificial fixing quantity of the gassiness preparation of soil sample.
The inventive method is by the special crystal structure of zeolite and strongly hydrophilic, and zeolite proportion is close with soil particle proportion, by the zeolite granular of the saturated methane gas of absorption and soil particle Homogeneous phase mixing, then add water, the methane gas adsorbed in zeolite granular is displaced with water, thus forming the bubbles soil body, gassiness soil sample prepared by the method is even.This method is applicable to the preparation of soil sample of coarse grained gassiness sand, is also suitable for the soft preparation of soil sample of fine grain gassiness.
Accompanying drawing explanation
Fig. 1 is the structural representation of a kind of transformation controllable gas displacement reaction device of the present invention.
Fig. 2 is the diagrammatic cross-section of reactor gland bonnet in a kind of transformation controllable gas displacement reaction device of the present invention.
Description of reference numerals is as follows: 1-water inlet, 2-water inlet pipe, 3-zeolite, 4-reactor, 5-reactor gland bonnet, 6-water inlet valve, 7-view window, 8-filtering head, 9-the first valve, 10-reactor tensimeter, 11-first row mouth of a river, 12-second row mouth of a river, 13-the second valve, 14-graduated cylinder tensimeter, 15-reactor intake and exhaust valve, 16-reactor porting, 17-withstand voltage drainage connecting pipe, 18-graduated cylinder porting, 19-graduated cylinder intake and exhaust valve, 20-graduated cylinder, 21-graduated cylinder gland bonnet, 22-scale, 23-indent cone-shaped space, 24-screw thread, 25-base.
Embodiment
Composition structure, the principle of work and methods for using them of apparatus of the present invention is introduced in detail below in conjunction with drawings and Examples.
Embodiment 1:
A kind of transformation controllable gas displacement reaction device, comprise reactor 4, graduated cylinder 20 and base 25, described reactor 4 and graduated cylinder 20 are fixed on the upper surface of base 25;
Described reactor 4 is prepared from by high pressure resistant material, and it is withstand voltage, and the limit is not less than 5MPa;
For ease of the level change of external observation reactor 4 inside, the sidewall of described reactor 4 is provided with vertical view window 7, and view window 7 is transparent resistance to laminated glass, is assembled into one with reactor 4, and keeps leakproofness and the resistance to pressure of whole reactor 4.
The upper end open of described reactor 4 and graduated cylinder 20, be stamped reactor gland bonnet 5 and graduated cylinder gland bonnet 21 respectively, further, reactor 4 and reactor gland bonnet 5 are threaded connection, graduated cylinder 20 and graduated cylinder gland bonnet 21 are also threaded connection, and ensure the airtight of reactor 4 and graduated cylinder 20;
The outside surface of described reactor gland bonnet 5 is plane, and inside surface is the taper shape of indent, in reactor gland bonnet 5, form an indent cone-shaped space 23, makes reactor gland bonnet 5 be the cover body structure of the thick intermediate thin in edge;
The conical top perforate of described reactor gland bonnet 5 inside surface indent, tapping establishes reactor porting 16, the pipeline of described reactor porting 16 is provided with reactor tensimeter 10, the opening part of described reactor porting 16 is provided with reactor intake and exhaust valve 15, reactor intake and exhaust valve 15 is discharged for controlling or is filled with gas in reactor 4, and 10, reactor tensimeter is for measuring the pressure in reactor 4;
Described reactor gland bonnet 5 is also provided with a water inlet 1 and two freeing port;
Described water inlet 1 is arranged at the side of reactor gland bonnet 5, described water inlet 1 place opens flat hole and is through to reactor gland bonnet 5 inside surface, the aperture place of inside surface is provided with water inlet pipe 2, water inlet pipe 2 passes from the indent cone-shaped space 23 in reactor gland bonnet 5 and puts in reactor 4, open the height of flat hole lower than the conical vertex of a cone of indent, like this reactor 4 inside is communicated with outside inlet pipeline, the pipeline at reactor gland bonnet 5 outer water inlet 1 place is provided with water inlet valve 6, water inlet valve 6 is for cutting off contacting of outside water inlet system and reactor 4 inside, the withstand voltage limit identical reaction kettle 4 of the water inlet pipe 2 in described reactor 4, also 5MPa is not less than,
Described two freeing port are respectively the first row mouth of a river 11 and the second row mouth of a river 12;
The described second row mouth of a river 12 is arranged at the opposite side of reactor gland bonnet 5, relative with described water inlet 1, the described second row mouth of a river 12 place opens flat hole and is through to reactor gland bonnet 5 inside surface, perforate is highly with water inlet 1, the aperture place of inside surface is provided with drainage pipe, described drainage pipe stretches to distance reactor 4 bottom surface 3cm or 4cm or 5cm place in reactor 4, drainage pipe is made up of filtering head 8 and pressure pipe, filtering head 8 is arranged at the lower end of pressure pipe, filtering head 8 is for filtering the solid particulate matter in reactor 4, guarantee the particulate matter can not taken away in the liquid of discharging in reactor 4, error is caused to test, the withstand voltage limit identical reaction kettle 4 of described pressure pipe, also 5MPa is not less than,
One end of the external withstand voltage drainage connecting pipe 17 in aperture, the second row mouth of a river 12 of reactor gland bonnet 5 outside, the other end of withstand voltage drainage connecting pipe 17 extends in graduated cylinder 20 through graduated cylinder gland bonnet 21, and described withstand voltage drainage connecting pipe 17 is provided with the second valve 13;
The described first row mouth of a river 11 is arranged on the sidewall of reactor gland bonnet 5, the described first row mouth of a river 11 is between water inlet and the second row mouth of a river 12, in the present embodiment, the described first row mouth of a river 11 and the second row mouth of a river 12 are arranged on the sidewall of reactor gland bonnet 5 in 90 °, the described first row mouth of a river 11 place opens flat hole, perforate height flushes with the conical vertex of a cone of the indent in reactor gland bonnet 5, flat hole is through to the vertex of a cone of reactor gland bonnet 5 inside surface, the pipeline at the first row mouth of a river 11 outside reactor gland bonnet 5 is provided with the first valve 9, for cutting off the passage of the outside overflow of liquid in reactor 4, the object of described reactor gland bonnet 5 structure like this is that liquid is input into after in airtight reactor 4 through water inlet 1, thoroughly can drain gas reactor, guarantee that reactor 4 inner space is all full of by liquid, not residual gas.
Graduated cylinder gland bonnet 21 is stamped due to described graduated cylinder 20 adding, therefore different from general uncovered graduated cylinder, for sealing graduated cylinder container, graduated cylinder 20 adopts withstand voltage transparent material to make cylindrical shape, barrel wall has worn lattice scale 22 for metered volume, the withstand voltage limit of graduated cylinder 20 is mated with reactor 4, is not less than 5MPa;
Described graduated cylinder gland bonnet 21 also offers a hole, this hole is connected with pipeline, one end of pipeline puts in graduated cylinder 20 by this hole, the other end is outside graduated cylinder 20, for graduated cylinder porting 18, this pipeline is provided with graduated cylinder tensimeter 14 and graduated cylinder intake and exhaust valve 19 successively along the direction that graduated cylinder is outwards vented, graduated cylinder tensimeter 14 is for measuring the pressure in graduated cylinder 20, and graduated cylinder intake and exhaust valve 19 is for controlling air inlet and exhaust.
In described transformation controllable gas displacement reaction device, each pipeline/road all needs to meet the extreme pressure requirement consistent with reactor 4 except voltage endurance capability, is namely all not less than beyond 5MPa, and the bore in each pipeline/road is unsuitable excessive, should select
Valve on each pipeline/road is without particular/special requirement, and with the match specifications in pipeline/road, the hole match specifications that the pipeline of each tapping is also all strict and corresponding, to ensure the leakproofness of whole device.
The device of the invention described above, when being applied in the gassiness preparation of soil sample, needs to carry out under constant indoor temperature condition.The present embodiment room temperature is set to 25 DEG C.
Be first 4 μm by the zeolite 3(white powder of specified particle diameter, particle diameter, intracrystalline pore footpath is 5 dusts (1 dust=10 -10m)) to insert in baking oven 105 DEG C and carry out the dry 24h that dewaters, then put into dry cylinder and cool.Under constant indoor temperature condition, take the zeolite 3 of certain mass, insert in reactor 4, cover reactor gland bonnet 5, close water inlet valve 6, first valve 9 at the first row mouth of a river 11 place, second valve 13 at the second row mouth of a river 12 place, open the reactor intake and exhaust valve 15 at reactor porting 16 place, the external vaccum-pumping equipment of reactor porting 16, vacuumizes reactor 4.Pressure-100kPa condition 24h is maintained, thoroughly to get rid of the air of reactor 4 and zeolite 3 absorption in reactor 4.The reactor intake and exhaust valve 15 at off-response still porting 16 place, open first valve 9 at the first row mouth of a river 11 place, the external introducing methane gas in the first row mouth of a river 11, make the pressure in reactor 4 for presetting adsorptive pressure (assumed stress value is A), pressure is shown by reactor tensimeter 10 and controls, the default adsorptive pressure (force value is A) maintained in reactor 4 is no less than 24h, and fully adsorbed methane gas is extremely saturated to make zeolite 3 energy.
A certain amount of degassed water is added in advance in graduated cylinder 20, open graduated cylinder air inlet and exhaust valve door 19, in the graduated cylinder 20 of sealing, inject difficult gas (as air, nitrogen etc.) to the pressure in graduated cylinder 20 being dissolved in water by graduated cylinder porting 18 and reach default adsorptive pressure (force value is A), pressure can be read by graduated cylinder tensimeter 14.In graduated cylinder 20, the initial volume reading of water reads by scale 22.
Open the water inlet valve 6 of reactor 4, by water inlet 1 external introducing degassed water (water temperature is consistent with constant indoor temperature temperature), degassed water is entered in reactor 4 by water inlet pipe 2.Control the suitable deflation rate of first valve 9 at the first row mouth of a river 11 place (can judge by the view window 7 place observation liquid level ascending velocity entered in reactor 4), degassed water is made in 2min, to fill rapidly whole reactor 4 inner space (if overlong time, larger test error can be caused), when the first row mouth of a river 11 place starts outside spilling water, rapid closedown first valve 9 and water inlet valve 6, continuing the pressure maintained in reactor 4 is default adsorption pressure force value (force value is A).
Open the second valve 13, water in reactor 4 displaces the methane gas of absorption in zeolite 3, gas collects at indent cone-shaped space 23 place of reactor gland bonnet 5, along with free gas constantly gathers, degassed water in reactor 4 enters the filtration of filtering head 8, flow through withstand voltage drainage connecting pipe 17 to enter in graduated cylinder 20, until displacement reaction stops (the displacement reaction time should be not less than 32h).Liquid level final volume is read from the scale 22 graduated cylinder 20, the difference of final volume and initial volume is the methane gas scale of construction (be converted into the gas flow under atmospheric pressure according to Boyle law, be convenient to the contrast of gas under pressure replacement amount at different levels) that the zeolite 3 of this quality displaces under this test pressure (force value is A).It is worth mentioning that, can jog test unit in displacement reaction process of the test, to make zeolite 3 and degassed water fully react, and the methane gas displaced is assembled under buoyancy to indent cone-shaped space 23 place at top.
By the force value in graduated cylinder air inlet and exhaust valve door 19 classification reduction graduated cylinder 20 (as force value A → B 1→ B 2→ B 3→ B 4, A > B 1> B 2> B 3> B 4), carry out displacement reaction continuously, same method can obtain different pressures, and (force value is B 1, B 2, B 3and B 4) under the replacement amount of methane gas, the quantitative relationship between the situation downforce of equal in quality zeolite and methane gas quantum of output can be set up thus.
According to above-mentioned method, then carry out the gas displacement reaction of different quality zeolite 3 under uniform pressure condition, the quantitative relationship between the quality of zeolite 3 under same pressure environment and methane gas quantum of output can be set up.
Thus, can realize under constant temperature by transformation controllable gas displacement reaction device experiment, different pressures environment, the measurement of quantitative relationship between zeolite 3 quality and gas quantum of output.According to the gas content wished to get in saturation degree gassiness soil, this species saturation gassiness soil of preparation can be gone out by inverse according to this quantitative relationship, the quality of zeolite 3 and required dry ground quality need be mixed.
Weigh the zeolite 3 of the drying cooling determining quality, make its methane adsorption saturated.Rapid taking-up zeolite 3 and in advance load weighted dry ground (clay, mean grain size D50 is about 4.5 μm) insert in airtight sample preparation device and carry out Homogeneous phase mixing, and pressure is the remoulded sample of predetermined dry density, this process need keep the pressure in airtight sample preparation device to be constant specified pressure (have nothing to do with preset pressure above, can freely specify) here.The pressure reduction keeping being not more than 5kPa is by degassed water from bottom to top submergence soil sample gradually bottom airtight sample preparation device, and the air in displacement soil pores is with saturated soil sample.Soil mesolite 3 particle meets the rearmounted methane gas that swaps out of water, thus is prepared into and can be used for predetermined saturation needed for indoor triaxial test and bubble distribution uniform gassiness soil soil sample.
Specific embodiment described in this instructions is only to the explanation for example of the present invention's spirit.Those skilled in the art can make various amendment or supplement or adopt similar mode to substitute to described specific embodiment, but can't depart from spirit of the present invention or surmount the scope that appended claims defines.

Claims (4)

1. a transformation controllable gas displacement reaction device, comprises reactor, graduated cylinder and base, and described reactor and graduated cylinder are fixed on base upper surface;
The sidewall of described reactor is provided with vertical view window, and view window is transparent material;
Described reactor and graduated cylinder upper end open, be stamped reactor gland bonnet and graduated cylinder gland bonnet respectively;
The outside surface of described reactor gland bonnet is plane, and inside surface is the taper shape of indent, in reactor gland bonnet, form an indent cone-shaped space;
The conical top perforate of described reactor gland bonnet inside surface indent, tapping establishes reactor porting, the pipeline of described reactor porting is provided with reactor tensimeter, and the opening part of described reactor porting is provided with reactor intake and exhaust valve;
Described reactor gland bonnet is also provided with a water inlet and two freeing port;
Described water inlet is arranged at the side of reactor gland bonnet, described water inlet is opened flat hole and is through to reactor gland bonnet inside surface, the aperture place of inside surface is provided with water inlet pipe, water inlet pipe passes from the indent cone-shaped space in reactor gland bonnet and puts in reactor, opens the conical vertex of a cone of height lower than indent of flat hole; The pipeline of the outer water inlet of reactor gland bonnet is provided with water inlet valve;
Described two freeing port are respectively the first row mouth of a river and the second row mouth of a river;
The described second row mouth of a river is arranged at the opposite side of reactor gland bonnet, relative with described water inlet, described second row mouth of a river place opens flat hole and is through to reactor gland bonnet inside surface, the highly same water inlet of perforate, the aperture place of inside surface is provided with drainage pipe, and described drainage pipe stretches to 3 ~ 5cm place, distance reactor bottom surface in reactor, and drainage pipe is made up of filtering head and pressure pipe, filtering head is arranged at the lower end of pressure pipe, and filtering head is for filtering the solid particulate matter in reactor;
One end of the external withstand voltage drainage connecting pipe in aperture, the second row mouth of a river of reactor gland bonnet outside, the other end of withstand voltage drainage connecting pipe extends in graduated cylinder through graduated cylinder gland bonnet, and described withstand voltage drainage connecting pipe is provided with the second valve;
The described first row mouth of a river is arranged on the sidewall of reactor gland bonnet, the described first row mouth of a river is between water inlet and the second row mouth of a river, described first row mouth of a river place opens flat hole, perforate height flushes with the conical vertex of a cone of the indent in reactor gland bonnet, flat hole is through to the vertex of a cone of reactor gland bonnet inside surface, and the pipeline at the first row mouth of a river outside reactor gland bonnet is provided with the first valve;
Described graduated cylinder gland bonnet also offers a hole, this hole is connected with pipeline, and one end of pipeline puts in graduated cylinder; The other end, outside graduated cylinder, is graduated cylinder porting; Pipeline is provided with graduated cylinder tensimeter and graduated cylinder intake and exhaust valve successively along discharge directions.
2. transformation controllable gas displacement reaction device according to claim 1, it is characterized in that: described reactor is prepared from by high pressure resistant material, it is withstand voltage, and the limit is not less than 5MPa; The withstand voltage limit identical reaction kettle of the water inlet pipe in described reactor, is also not less than 5MPa; The withstand voltage limit identical reaction kettle of described pressure pipe, is also not less than 5MPa; Graduated cylinder is withstand voltage, and the limit is mated with reactor, is not less than 5MPa.
3. the application of transformation controllable gas displacement reaction device in the gassiness preparation of soil sample described in claim 1 or 2.
4. utilize the transformation controllable gas displacement reaction device described in claim 1 or 2 to prepare a method for gassiness soil sample, its step is as follows:
(1) zeolite granular of selected particle diameter is inserted in baking oven carry out drying and dewater, then put into dry cylinder to cool, under constant indoor temperature condition, take the zeolite granular of the drying cooling of certain mass, insert in reactor and vacuumized by reactor porting, get rid of the air adsorbed in reactor and in zeolite granular, then in reactor, passing into the methane gas of test predetermined pressure by the first row mouth of a river, to carry out absorption saturated, saturated complete after, be rapidly in reactor by water inlet and pass into degassed water until be all full of by water in still, not residual gas, after being filled with the air of test predetermined pressure in graduated cylinder, open the second valve between graduated cylinder and reactor, water in reactor displaces the methane gas adsorbed in zeolite granular, gas converges gradually at reactor top conical shape top, and the water in reactor is under gas pressure, flowed in graduated cylinder until test stops by drainage pipe, flow into the volume of water in graduated cylinder and be the methane gas scale of construction that the zeolite of this certain mass displaces under this test pressure,
(2) carry out the gas displacement reaction of different quality zeolite granular under uniform pressure condition according to step (1), the quantitative relationship between zeolite granular quality and gas quantum of output under same pressure environment can be set up out; Carry out the gas displacement reaction of zeolite granular under different pressures condition of equal in quality again, the quantitative relationship between pressure and gas quantum of output can be set up out; Thus, undertaken under test can set up constant temperature by described transformation controllable gas displacement reaction device, pressure, quantitative relationship between zeolite granular quality and gas quantum of output; According to gas flow contained in the gassiness soil wishing to get saturation degree, the quality of zeolite granular and required dry ground quality can should be mixed by the inverse gassiness soil that goes out this saturation degree of preparation according to above-mentioned quantitative relationship;
(3) zeolite granular cooled by the drying determining quality in step (2) is weighed, insert closed container to vacuumize, at least 24h is preserved under-100kPa pressure, and in backward closed container, be filled with the methane gas of predetermined pressure, deposit at least 24h saturated to methane adsorption, rapid taking-up zeolite granular, insert in the lump in airtight sample preparation device with load weighted dry ground in advance and mix, complete from taking-up zeolite granular to the 2-5min that operates in mixed, and be set to the remoulded sample of default dry density, this process need keep the pressure in airtight sample preparation device to be constant specified pressure, the pressure reduction keeping being not more than 5kPa is by degassed water from bottom to top submergence soil sample gradually bottom airtight sample preparation device, air in displacement soil mesoporosity is with saturated soil sample, soil mesolite particle meets the rearmounted methane gas that swaps out of water, thus be prepared into and can be used for predetermined saturation needed for indoor triaxial test and bubble distribution uniform gassiness soil soil sample.
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