CN111337337A - Variable-density gas-containing soil sample preparation device and method based on zeolite displacement reaction - Google Patents
Variable-density gas-containing soil sample preparation device and method based on zeolite displacement reaction Download PDFInfo
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- CN111337337A CN111337337A CN202010203798.5A CN202010203798A CN111337337A CN 111337337 A CN111337337 A CN 111337337A CN 202010203798 A CN202010203798 A CN 202010203798A CN 111337337 A CN111337337 A CN 111337337A
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- 239000002689 soil Substances 0.000 title claims abstract description 325
- 239000010457 zeolite Substances 0.000 title claims abstract description 92
- 229910021536 Zeolite Inorganic materials 0.000 title claims abstract description 91
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 title claims abstract description 88
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 238000000034 method Methods 0.000 title claims abstract description 14
- 238000006073 displacement reaction Methods 0.000 title claims abstract description 10
- 238000006243 chemical reaction Methods 0.000 claims abstract description 97
- 239000002002 slurry Substances 0.000 claims abstract description 65
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 59
- 238000007789 sealing Methods 0.000 claims description 39
- 239000000463 material Substances 0.000 claims description 34
- 238000003756 stirring Methods 0.000 claims description 24
- 239000000843 powder Substances 0.000 claims description 20
- 238000003860 storage Methods 0.000 claims description 15
- 238000012360 testing method Methods 0.000 claims description 11
- 239000012153 distilled water Substances 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 10
- 230000008014 freezing Effects 0.000 claims description 9
- 238000007710 freezing Methods 0.000 claims description 9
- 239000011148 porous material Substances 0.000 claims description 8
- 238000005303 weighing Methods 0.000 claims description 7
- 239000004575 stone Substances 0.000 claims description 6
- 230000005484 gravity Effects 0.000 claims description 5
- 238000009434 installation Methods 0.000 claims description 5
- 230000009471 action Effects 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 230000000149 penetrating effect Effects 0.000 claims description 4
- 229920006395 saturated elastomer Polymers 0.000 claims description 4
- 238000007493 shaping process Methods 0.000 claims description 4
- 238000005086 pumping Methods 0.000 claims description 3
- 238000006467 substitution reaction Methods 0.000 claims 6
- 238000002474 experimental method Methods 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 238000002347 injection Methods 0.000 description 3
- 239000007924 injection Substances 0.000 description 3
- 239000013049 sediment Substances 0.000 description 3
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 241000121220 Tricholoma matsutake Species 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000012669 compression test Methods 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000009740 moulding (composite fabrication) Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000004088 simulation Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/36—Embedding or analogous mounting of samples
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/38—Diluting, dispersing or mixing samples
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/38—Diluting, dispersing or mixing samples
- G01N2001/386—Other diluting or mixing processes
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N2203/02—Details not specific for a particular testing method
- G01N2203/026—Specifications of the specimen
- G01N2203/0298—Manufacturing or preparing specimens
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Abstract
The invention discloses a variable-density gas-containing soil sample preparation device and method based on zeolite displacement reaction, and the device comprises a zeolite reaction kettle, a soil sample reaction kettle and a soil sample forming box, wherein the bottom of the zeolite reaction kettle is communicated with the middle part of the soil sample reaction kettle through a high-pressure conduit A, the top of the zeolite reaction kettle is communicated with an air inlet pipe B and a first vacuum pressure gauge, the top of the soil sample reaction kettle is communicated with the bottom of the soil sample forming box through the high-pressure conduit B, a stirrer is correspondingly arranged in the soil sample reaction kettle, the top of the soil sample reaction kettle is communicated with the air inlet pipe A and the second vacuum pressure gauge, the bottom of the soil sample reaction kettle is communicated with an water inlet pipe, the bottom of the soil sample reaction kettle is communicated with the top of the soil sample forming box through a soil slurry communicating pipe, and the soil slurry communicating pipe is sequentially provided with a fourth valve; and a third vacuum pressure gauge is communicated with the bottom of the soil sample forming box. The invention can prepare the gas-containing soil sample which is not limited by density conditions and meets the requirements of indoor geotechnical experiments in a batch and controllable manner.
Description
Technical Field
The invention relates to the technical field of geotechnical engineering geotechnical tests, in particular to a device and a method for preparing a variable-density gas-containing soil sample based on zeolite displacement reaction, and particularly relates to an indoor artificial simulation sample preparation technology for seabed gas-containing sediments.
Background
The gas-containing soil is particularly the soil body with gas in a closed free and dissolved state rather than a gas-water compound state. It is considered to be a metastable state balancing body composed of soil particles, pore water, gas, temperature and overlying layer pressure, and once the balance is broken, the engineering properties of the metastable state balancing body can be rapidly changed, thus causing disasters to the engineering. Such as: the gas-containing sediments on the seabed often cause disastrous accidents such as coast landslide, soil liquefaction, foundation settlement and the like, and are important potential safety hazards in ocean engineering.
The gas-containing soil generally exists in nature, but the gas pressure in the soil is large and unstable, so that the decomposition, desolventization and dissipation are easy, the original structure of the soil is damaged, and the field original gas-containing soil sample is difficult to obtain. Even if special equipment is adopted to obtain a pressure-maintaining undisturbed soil sample, the problems of difficult secondary processing indoors, uneven gas content of the soil sample and the like still exist, so that the development of an indoor method for manually preparing gas-containing soil is promoted, and the engineering characteristics of seabed gas-containing sediments are researched by simulating the preparation of the gas-containing soil sample. The patent ZL201310752757.1 provides a method for forming gas-containing soil by replacing zeolite with water to adsorb methane gas by virtue of zeolite adsorption property, but the method is only suitable for preparing gas-containing soil samples of loose tricholoma matsutake, but cannot be prepared for preparing gas-containing soil samples with higher density.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a variable-density gas-containing soil sample preparation device and method based on zeolite displacement reaction, which are used for displacing N in zeolite by using water in sample pores2Gas, mixing with N by zeolite powder2Gas content through respective flow ratesMeasuring the ratio to obtain the soil slurry with accurate data, introducing the measured soil slurry into a soil sample forming box, obtaining a soil sample with the required sample height through a material pushing piston with scales, freezing and forming, melting under the back pressure of less than or equal to 200kPa, and replacing N in zeolite by soil sample pore water2And (5) gas, thus preparing gas-containing soil samples with different densities.
The purpose of the invention is realized by the following technical scheme:
a variable-density gas-containing soil sample preparation device based on zeolite displacement reaction comprises a zeolite reaction kettle, a soil sample reaction kettle and a soil sample forming box, wherein the bottom of the zeolite reaction kettle is communicated with the middle part of the soil sample reaction kettle through a high-pressure guide pipe A, the top of the zeolite reaction kettle is communicated with an air inlet pipe B and a first vacuum pressure gauge, and the air inlet pipe B is provided with a first valve; the top of the soil sample reaction kettle is communicated with the bottom of the soil sample forming box through a high-pressure guide pipe B, a third valve is arranged at the position, close to the top of the soil sample reaction kettle, of the high-pressure guide pipe B, and an eighth valve is arranged at the position, close to the bottom of the soil sample forming box, of the high-pressure guide pipe B; the soil sample reaction kettle is correspondingly provided with a stirrer, the top of the soil sample reaction kettle is communicated with an air inlet pipe A and a second vacuum pressure gauge, the air inlet pipe A is provided with a fifth valve, and the soil sample reaction kettle is internally provided with a thermometer; the bottom of the soil sample reaction kettle is communicated with a water inlet pipe, and a second flowmeter and a sixth valve are correspondingly arranged on the water inlet pipe; the bottom of the soil sample reaction kettle is communicated with the top of the soil sample forming box through a soil slurry communicating pipe, and a fourth valve, a first flowmeter and a seventh valve are sequentially arranged on the soil slurry communicating pipe from top to bottom; soil sample shaping box bottom intercommunication is equipped with third vacuum pressure table, soil sample shaping box includes mould top cap, moulded die and mould bottom cap, the detachable seal installation in moulded die top of mould top cap, the detachable seal installation in moulded die bottom, the mould top cap is equipped with the material piston that pushes away of taking the scale.
In order to better realize the method, the zeolite reaction kettle comprises a tank body and a zeolite sealing cover which is hermetically covered at a tank opening at the top of the tank body, wherein the zeolite sealing cover and the top of the tank body are fixedly connected through a plurality of first bolts; the bottom of the tank body is in a funnel shape, a second valve is arranged at the position, close to the bottom of the tank body, of the high-pressure guide pipe A, and the air inlet pipe B and the first vacuum pressure gauge are communicated and arranged on the zeolite sealing cover.
Preferably, the material pushing piston comprises a material pushing rod, a material pushing handle and a material pushing piston plate, the material pushing rod is installed on the die top cover in a penetrating mode, the material pushing handle is fixed to the top end of the material pushing rod, the material pushing piston plate is fixed to the bottom end of the material pushing rod, the material pushing piston plate is located inside the forming die in a matched mode, the material pushing handle is located outside the soil sample forming box, and the material pushing rod is provided with scale marks along the height direction.
Preferably, the soil sample reaction kettle comprises a cylinder body and a soil sample sealing cover which is hermetically covered on a cylinder opening at the top of the cylinder body, and the soil sample sealing cover and the top of the cylinder body are fixedly connected through a plurality of second bolts; the air inlet pipe A and the second vacuum pressure gauge are communicated with each other and arranged on the soil sample sealing cover, and the end part of the high-pressure guide pipe B is communicated with and arranged on the soil sample sealing cover.
Preferably, the invention also comprises a vacuum pump and N2The vacuum pump is provided with an evacuation pipe, the evacuation pipe of the vacuum pump corresponds to the air inlet pipe A and the air inlet pipe B respectively, and N is2The storage tank is provided with an air outlet pipe, N2The air outlet pipe of the storage tank corresponds to the air inlet pipe A and the air inlet pipe B respectively.
Preferably, the agitator includes agitator motor, (mixing) shaft and stirring rake, the (mixing) shaft rotates to run through and installs on soil sample closing cap, the cooperation is installed a plurality of stirring rake on the (mixing) shaft, and all stirring rakes all are located the barrel inside, agitator motor installs on soil sample closing cap, agitator motor's power output shaft and (mixing) shaft power are connected.
Preferably, the end part of the high-pressure conduit B is communicated with and arranged on the mold bottom cover, the bottom end of the slurry communicating pipe is communicated with and arranged on the mold top cover, and the third vacuum pressure gauge is communicated and arranged at the bottom of the forming mold.
A method for preparing a variable-density gas-containing soil sample based on zeolite displacement reaction comprises the following steps:
A. placing saturated permeable stone and filter paper on the mould bottom cover in turn from bottom to top, sealing the forming mould through the mould top cover and the mould bottom cover to form a closed soil sample forming box, and weighing the mass m of the soil sample forming box at the moment0(ii) a Installing a soil sample reaction kettle, wherein the mass is m1The dried soil is put into the cylinder body, and a soil sample sealing cover is closed; installing a zeolite reaction kettle, wherein the mass is m1The dried zeolite powder is put into a zeolite reaction kettle, and a zeolite sealing cover is closed;
B. communicating the zeolite reaction kettle and the soil sample reaction kettle through a high-pressure conduit A, communicating the soil sample reaction kettle and the soil sample forming box through a high-pressure conduit B, hermetically communicating a vacuumizing pipe of a vacuum pump with an air inlet pipe A and an air inlet pipe B respectively, closing a fourth valve and a sixth valve, opening a first valve, a third valve, a fifth valve, a seventh valve and an eighth valve, and starting the vacuum pump to exhaust air in the zeolite reaction kettle, the soil sample forming box and the dried soil; when the first vacuum pressure gauge, the second vacuum pressure gauge and the third vacuum pressure gauge are close to-100 kPa, continuously pumping air for not less than 1.5 hours, and then closing the first valve and the fifth valve;
C. respectively connecting an air inlet pipe A and an air inlet pipe B with high purity N2Storage tank, adjusting N2A pressure reducing valve of the storage tank to maintain the pressure at 300 kPa; opening the first valve and the fifth valve, closing the first valve and the fifth valve after the first vacuum pressure gauge and the second vacuum pressure gauge are stabilized at 300kPa, and standing for 12 hours while keeping the pressure not to be obviously reduced;
D. opening a second valve to enable all zeolite powder in the tank body to fall into the soil sample reaction kettle, then closing the second valve and opening a stirrer for stirring operation to enable dried soil and zeolite powder to be uniformly mixed, and recording the temperature value of the thermometer;
E. immersing the water inlet pipe into the distilled water in the water injection tank, opening the sixth valve to ensure that the distilled water is slowly injected into the cylinder body from the water inlet pipe, and recording the flow reading V on the second flowmeter0Closing the sixth valve; the stirrer is opened for stirring, so that the soil and the water are uniformly mixed to form soil slurry；
F. Opening the fourth valve and the seventh valve, allowing the soil slurry in the soil sample reaction kettle to flow into the soil sample forming box under the action of gravity, recording the flow through the first flowmeter, and closing the seventh valve after the required soil slurry flows into the soil sample forming box;
G. opening the eighth valve, and slowly pushing the pushing piston by using a jack to solidify and deform the soil slurry until the sample height of the required soil sample is reached; standing and closing the eighth valve after the water head discharged into the high-pressure conduit B is stable and unchanged and exceeds 24 hours; removing the soil slurry communicating pipe and the high-pressure guide pipe B, and integrally moving the soil sample forming box into a freezing chamber for freezing and forming; after forming, unscrewing a mold bottom cover of the soil sample forming box, pushing out the soil sample through a material pushing piston, and quickly installing the soil sample on a base of the triaxial apparatus for geotechnical engineering; controlling the back pressure to be less than or equal to 200kPa through a triaxial test system; after the soil sample is melted, the water in the pores of the soil sample is slowly replaced by the N in the zeolite2Qi until stable.
Compared with the prior art, the invention has the following advantages and beneficial effects:
(1) the device can be used for preparing the gas-containing soil samples with different densities which are not limited by density conditions and meet the requirements of indoor geotechnical experiments in batches and quantitatively.
(2) The sample preparation device replaces N in zeolite by water in sample pores2Gas, mixing with N by zeolite powder2And (3) gas content, namely, proportioning the soil slurry to obtain accurate data through each flowmeter, then introducing the metered soil slurry into a soil sample forming box, solidifying and deforming the soil slurry through a material pushing piston with scales to obtain a soil sample with the required sample height, and preparing gas-containing soil samples with different densities.
(3) The invention has wide applicable soil types, is not only applicable to coarse-grained sandy soil, but also applicable to fine-grained cohesive soil, and is not limited by the density condition of the prepared sample; meanwhile, the device has the advantages of uniform gas content of the soil sample, repeatable sample preparation, high manufacturing efficiency, convenient installation of the device and low cost.
(4) According to the invention, by replacing the soil sample forming boxes with different sizes, the gas-containing soil samples (such as one-dimensional compression test, triaxial test, cyclic shear test and the like) required by various soil tests can be prepared, and the method is suitable for preparing the gas-containing soil samples in batches in a short time and is used for researching different mechanical properties of the gas-containing soil in the soil tests.
Drawings
FIG. 1 is a schematic structural view of the present invention;
FIG. 2 is a schematic diagram of the structure of the zeolite reactor of FIG. 1.
Wherein, the names corresponding to the reference numbers in the drawings are:
1-zeolite reaction kettle, 100-first valve, 101-first vacuum pressure gauge, 102-zeolite sealing cover, 103-first bolt, 104-zeolite powder, 105-tank, 106-second valve, 107-high pressure conduit A, 108-air inlet pipe B, 2-soil sample reaction kettle, 200-thermometer, 201-third valve, 202-second bolt, 203-soil sample sealing cover, 204-stirrer, 205-cylinder, 206-soil sample, 207-fourth valve, 208-first flowmeter, 209-second vacuum pressure gauge, 210-fifth valve, 211-air inlet pipe A, 212-second flowmeter, 213-water inlet pipe, 214-sixth valve, 215-high pressure conduit B, 3-soil sample forming box, 300-seventh valve, 301-mold top cover, 302-forming mold, 303-filter paper, 304-mold bottom cover, 305-eighth valve, 306-graduation line, 307-pushing piston, 308-third vacuum pressure gauge, 309-permeable stone and 4-soil slurry communicating pipe.
Detailed Description
The present invention will be described in further detail with reference to the following examples:
example one
As shown in fig. 1-2, a variable density gas-containing soil sample preparation device based on zeolite displacement reaction comprises a zeolite reaction kettle 1, a soil sample reaction kettle 2 and a soil sample forming box 3, wherein the bottom of the zeolite reaction kettle 1 is communicated with the middle of the soil sample reaction kettle 2 through a high-pressure conduit A107, the top of the zeolite reaction kettle 1 is communicated with an air inlet pipe B108 and a first vacuum pressure gauge 101, and the air inlet pipe B108 is provided with a first valve 100. The top of the soil sample reaction kettle 2 is communicated with the bottom of the soil sample forming box 3 through a high-pressure guide pipe B215, a third valve 201 is arranged at the position, close to the top of the soil sample reaction kettle 2, of the high-pressure guide pipe B215, and an eighth valve 305 is arranged at the position, close to the bottom of the soil sample forming box 3, of the high-pressure guide pipe B215. The stirrer 204 is correspondingly installed in the soil sample reaction kettle 2, the top of the soil sample reaction kettle 2 is communicated with an air inlet pipe A211 and a second vacuum pressure gauge 209, the air inlet pipe A211 is provided with a fifth valve 210, and the soil sample reaction kettle 2 is internally provided with a thermometer 200. The bottom of the soil sample reaction kettle 2 is communicated with a water inlet pipe 213, and a second flowmeter 212 and a sixth valve 214 are correspondingly arranged on the water inlet pipe 213. The bottom of the soil sample reaction kettle 2 is communicated with the top of the soil sample forming box 3 through a soil slurry communicating pipe 4, and the soil slurry communicating pipe 4 is sequentially provided with a fourth valve 207, a first flowmeter 208 and a seventh valve 300 from top to bottom. The bottom of the soil sample forming box 3 is communicated with a third vacuum pressure gauge 308, the soil sample forming box 3 comprises a mold top cover 301, a forming mold 302 and a mold bottom cover 304, the mold top cover 301 is detachably and hermetically mounted at the top of the forming mold 302, the mold bottom cover 304 is detachably and hermetically mounted at the bottom of the forming mold 302, and the mold top cover 301 is provided with a material pushing piston 307 with scales. The soil sample forming box 3 is internally provided with a permeable stone 309 and filter paper 303 from bottom to top in sequence. The end of the high-pressure conduit B215 is communicated with and arranged on the die bottom cover 304, the bottom end of the slurry communicating pipe 4 is communicated with and arranged on the die top cover 301, and the third vacuum pressure gauge 308 is communicated with and arranged at the bottom of the forming die 302.
As shown in fig. 1 and 2, the zeolite reaction kettle 1 includes a tank 105 and a zeolite sealing cover 102 hermetically covering a tank opening at the top of the tank 105, and the zeolite sealing cover 102 is further fixedly connected to the top of the tank 105 by a plurality of first bolts 103. The bottom of the tank body 105 is in a funnel shape, a second valve 106 is arranged at the position, close to the bottom of the tank body 105, of the high-pressure guide pipe A107, and the air inlet pipe B108 and the first vacuum pressure gauge 101 are communicated and arranged on the zeolite sealing cover 102.
As shown in fig. 1, the pushing piston 307 includes a pushing rod, a pushing handle, and a pushing piston plate, the pushing rod is mounted on the mold top cover 301 in a penetrating manner, the pushing handle is fixed to the top end of the pushing rod, the pushing piston plate is fixed to the bottom end of the pushing rod, the pushing piston plate is located inside the forming mold 302 in a matching manner, the pushing handle is located outside the soil sample forming box 3, and the pushing rod is provided with a scale mark 306 along the height direction.
As shown in fig. 1, the soil sample reaction kettle 2 comprises a cylinder 205 and a soil sample sealing cover 203 hermetically covering the top opening of the cylinder 205, and the soil sample sealing cover 203 and the top of the cylinder 205 are further connected and fixed through a plurality of second bolts 202. The air inlet pipe A211 and the second vacuum pressure gauge 209 are communicated and arranged on the soil sample sealing cover 203, and the end part of the high-pressure conduit B215 is communicated and arranged on the soil sample sealing cover 203.
The invention also comprises a vacuum pump and N2A storage tank and a water injection tank, wherein the vacuum pump is provided with an evacuating pipe, the evacuating pipe of the vacuum pump corresponds to the air inlet pipe A211 and the air inlet pipe B108 respectively, and N is2The storage tank has an outlet pipe, N2The air outlet pipe of the storage tank corresponds to the air inlet pipe A211 and the air inlet pipe B108 respectively.
As shown in fig. 1, a preferred stirrer 204 of the present invention includes a stirring motor, a stirring shaft and stirring paddles, wherein the stirring shaft is rotatably installed on the soil sample sealing cover 203 in a penetrating manner, the stirring shaft is cooperatively installed with a plurality of stirring paddles, all the stirring paddles are located inside the cylinder 205, the stirring motor is installed on the soil sample sealing cover 203, and a power output shaft of the stirring motor is in power connection with the stirring shaft.
A method for preparing a variable-density gas-containing soil sample based on zeolite displacement reaction comprises the following steps:
A. placing saturated permeable stone 309 and filter paper 303 on the mold bottom cover 304 from bottom to top in sequence, sealing the forming mold 302 through the mold top cover 301 and the mold bottom cover 304 to form a closed soil sample forming box 3, and weighing the mass m of the soil sample forming box 3 at the moment0. Installing a soil sample reaction kettle 2 with mass m1The dried soil is put into a cylinder 205, and a soil sample sealing cover 203 is sealed and covered. The zeolite reaction kettle 1 is arranged, and the mass is m1The dried zeolite powder 104 is put into the zeolite reaction kettle 1, and the zeolite sealing cover 102 is closed and covered.
B. Communicating a zeolite reaction kettle 1 with a soil sample reaction kettle 2 through a high-pressure conduit A107, communicating the soil sample reaction kettle 2 with a soil sample forming box 3 through a high-pressure conduit B215, hermetically communicating a vacuum pumping pipe of a vacuum pump with an air inlet pipe A211 and an air inlet pipe B108 respectively, closing a fourth valve 207 and a sixth valve 214, opening a first valve 100, a third valve 201, a fifth valve 210, a seventh valve 300 and an eighth valve 305, and starting the vacuum pump to completely pump air in the zeolite reaction kettle 1, the soil sample reaction kettle 2, the soil sample forming box 3 and dried soil; when the first vacuum pressure gauge 101, the second vacuum pressure gauge 209 and the third vacuum pressure gauge 308 are all close to-100 kPa, the air suction is continued for not less than 1.5 hours, and then the first valve 100 and the fifth valve 210 are closed.
C. Respectively connecting an air inlet pipe A211 and an air inlet pipe B108 with high-purity N2Storage tank, adjusting N2The pressure reduction valve of the storage tank maintained the pressure at 300 kPa. The first valve 100 and the fifth valve 210 are opened, after the first vacuum pressure gauge 101 and the second vacuum pressure gauge 209 are stabilized at 300kPa, the first valve 100 and the fifth valve 210 are closed, and the mixture is placed for 12 hours and the pressure is kept not to be obviously reduced.
D. And opening the second valve 106 to enable all the zeolite powder 104 in the tank body 105 to fall into the soil sample reaction kettle 2, then closing the second valve 106 and opening the stirrer 204 for stirring operation, so that the dried soil and the zeolite powder 104 are uniformly mixed, and recording the temperature value of the thermometer 200.
E. Submerging the inlet tube 213 into the distilled water in the tank, opening the sixth valve 214 to allow the distilled water to be slowly injected into the barrel 205 through the inlet tube 213, and recording the flow reading V on the second flow meter 2120The sixth valve 214 is closed. The stirrer 204 is turned on to stir, so that the soil and the water are uniformly mixed to form soil slurry.
F. And (3) opening the fourth valve 207 and the seventh valve 300, allowing the soil slurry in the soil sample reaction kettle 2 to flow into the soil sample forming box 3 under the action of gravity, recording the flow through the first flow meter 208, and closing the seventh valve 300 after the required soil slurry flows into the soil sample forming box 3.
G. Opening the eighth valve 305, and slowly pushing the pushing piston 307 by using the jack to solidify and deform the soil slurry until the sample height of the required soil sample 206 is reached; standing and closing the eighth valve 305 after the water head discharged into the high-pressure conduit B215 is stable and constant and exceeds 24 hours; and (4) removing the soil slurry communicating pipe 4 and the high-pressure guide pipe B215, and integrally moving the soil sample forming box 3 into a freezing chamber for freezing and forming. After the forming, the mold bottom cover 304 of the soil sample forming box 3 is unscrewed, the soil sample 206 is pushed out through the material pushing piston 307, and the soil sample 206 is quickly installedThe device is arranged on a base of the geotechnical triaxial apparatus; controlling the back pressure to be less than or equal to 200kPa through a triaxial test system; after the soil sample is melted, the water in the pores of the soil sample 206 slowly replaces the N adsorbed in the zeolite powder2Qi until stable.
Example two
In this example, submarine clay (particle size less than 0.075mm and maximum specific gravity Gs of 2.73) was used as the target to prepare gas-containing soil according to the zeolite replacement principle disclosed in the patent "pressure swing controllable gas replacement reaction apparatus and its application in preparation of gas-containing soil sample (patent No. ZL 201310752757.1)", and the amount of zeolite added was 5% to prepare different initial densities (as experimental requirements: dry densities of 1.60g/cm respectively)3、1.65g/cm3And 1.70g/cm3) The aerated soft soil triaxial soil sample (experimental requirements are: diameter d of 50mm, height h of 100mm, and volume of 196.34cm3) The method can also be applied to the preparation of aerated soft soil triaxial soil samples required by other geotechnical experiments; the test is carried out in a constant-temperature indoor environment, and the specific sample preparation is carried out according to the following steps:
first step, device Assembly
(1) Sealing the forming mold 302 with a mold top cover 301 and a mold bottom cover 304 to form a closed soil sample forming box 3, placing a saturated permeable stone 308 and a filter paper 303 on the mold bottom cover 303 from bottom to top in sequence, and weighing the mass m of the empty soil sample forming box 30Namely:
m0＝2620.66g
(2) the zeolite reaction kettle 1 and the soil sample reaction kettle 2 are hermetically communicated by a high-pressure conduit A107, the soil sample reaction kettle 2 and the soil sample forming box 3 are hermetically communicated by a high-pressure conduit B215, the fourth valve 207 and the sixth valve 214 are closed, and the first valve 100, the third valve 201, the fifth valve 210, the seventh valve 300 and the eighth valve 305 are opened.
Second step, sample preparation
(1) Weighing 4750g of dried soil and placing the dried soil into a soil sample reaction kettle 2, weighing 250g of dried zeolite powder 104 and placing the dried zeolite powder 104 into a zeolite reaction kettle 1, wherein the mass of the mixed soil formed by the dried soil and the zeolite powder 104 is 4750g +250 g-5000 g, namely 5 kg; the top of the zeolite reaction kettle 1 is covered with a zeolite sealing cover 102, and is screwed with a first bolt 103 for sealing and fixing, and the top of the soil sample reaction kettle 2 is covered with a soil sample sealing cover 202, and is screwed with a second bolt 202 for sealing and fixing.
(2) The vacuumizing pipe of the vacuum pump is hermetically communicated with an air inlet pipe A211 and an air inlet pipe B108 respectively, the fourth valve 207 and the sixth valve 214 are closed, the first valve 100, the third valve 201, the fifth valve 210, the seventh valve 300 and the eighth valve 305 are opened, the vacuum pump is started to exhaust air in the zeolite reaction kettle 1, the soil sample reaction kettle 2 and the soil sample forming box 3, when the first vacuum pressure gauge 101, the second vacuum pressure gauge 209 and the third vacuum pressure gauge 308 are close to-100 kPa, the air is continuously exhausted for not less than 1.5 hours, and then the first valve 100 and the fifth valve 210 are closed.
(3) Respectively connecting an air inlet pipe A211 and an air inlet pipe B108 with high-purity N2Storage tank, adjusting N2A pressure reducing valve of the storage tank to maintain the pressure at 300 kPa; the first valve 100 and the fifth valve 210 are opened, after the first vacuum pressure gauge 101 and the second vacuum pressure gauge 209 are stabilized at 300kPa, the first valve 100 and the fifth valve 210 are closed, and the mixture is placed for 12 hours and the pressure is kept not to be obviously reduced.
(4) Opening the second valve 106 to enable all the zeolite powder 104 in the tank body 105 to fall into the soil sample reaction kettle 2, closing the second valve 106, opening the stirrer 204, and then stirring to enable the dried soil and the zeolite powder 104 to be uniformly mixed; the stirrer 209 was stopped and the temperature value of the thermometer 200 was recorded as 25 ℃ (room temperature).
(5) Distilled water (density ρ of distilled water) in which water inlet pipe 213 is immersed in water tankWater (W)Is 1g/cm3) In the middle, the sixth valve 214 is opened to make the distilled water in the water filling tank slowly fill the cylinder 205 through the water inlet pipe 213, and the flow reading V on the second flow meter 212 is recorded0，V0At 5L, the sixth valve 214 is closed; turning on the stirrer 204 for stirring to uniformly mix the soil and the water to form soil slurry;
distilled water flow rate V recorded by the second flow meter 2120＝5L；
According to the formula mWater (W)＝V0×ρWater (W)Calculating to obtain the mass m of water injectionWater (W)＝5kg：
Thirdly, forming a soil sample
(1) Determining slurry density
Opening the fourth valve 207 and the seventh valve 300, allowing the soil slurry in the soil sample reaction kettle 2 to flow into the soil sample forming box 3 under the action of gravity, recording the flow rate through the first flow meter 208 (zero clearing before use), and closing the seventh valve 300 when the reading of the first flow meter 208 is 100 ml;
at this time, the volume V of the slurry entering the forming mold 302 from the cylinder 2052＝100cm3；
(2) Weighing the sample box 3 and the internal soil slurry to obtain the total mass m1：
m1＝2796.11g
(3) Calculating the density rho of the soil slurry according to a density rho formula in soil mechanics, namely:
wherein rho is the density (g/cm) of the slurry3)；
m-mass of the slurry (g);
v-volume of soil slurry (cm)3)。
Mass m of the slurry is m1-m02796.11-2620.66-175.45 g, volume V of slurry2＝100cm3The density rho of the slurry is 175.45 ÷ 100 ÷ 1.7545g/cm3(i.e., slurry density ρ)Pulp and its production processIs 1.7545g/cm3)。
And calculating the water content w of the soil slurry according to a water content w formula, namely:
in the formula, w is the water content of the soil slurry;
mw-mass of water (g);
ms-mass of dry soil (g).
Mass m of waterw＝mWater (W)＝V0×ρWater (W)＝5kg，ms4750g +250 g-5000 g-5 kg, and the water content w of the obtained soil slurry is 100%.
According to dry density ρdCalculating the dry density rho of the soil slurry by a formuladNamely:
ρd＝ρ/(1+w)；
density of slurry rhoPulp and its production processIs 1.7545g/cm3Dry density ρdIs 0.877g/cm3Dry density ρdReserving three digits after decimal point;
by dry density ρdIs 0.877g/cm3Respectively preparing soil slurry with the water content w of 100 percent into soil slurry with the dry density of 1.60g/cm3、1.65g/cm3And 1.70g/cm3The aerated soft soil triaxial soil sample (diameter d is 50mm, height h is 100mm, volume V)2Is 196.34cm3) According to the density formula md＝ρd× V, the mass of the dry soil (two figures after calculating and reserving decimal point) required for obtaining the three different densities is respectively:
the dry density was 1.60g/cm3Dry soil mass m required by aerated soft soil triaxial soil sampled1＝V2×1.60＝314.14g，
The dry density was 1.65g/cm3Dry soil mass m required by aerated soft soil triaxial soil sampled2＝V2×1.65＝324.16g，
The dry density was 1.70g/cm3Dry soil mass m required by aerated soft soil triaxial soil sampled3＝V2×1.70＝333.78g，
Wherein m isd1、md2、md3Respectively has a dry density of 1.60g/cm3、1.65g/cm3And 1.70g/cm3The corresponding dry soil mass is m according to the mass formulad(1+ w) required slurry (dry density ρ)dIs 0.877g/cm3The slurry having a water content w of 100%, which was prepared as described above in this example) was:
the dry density was 1.60g/cm3The soil slurry mass m required by the aerated soft soil triaxial soil sample2＝md1×2＝628.28g，
The dry density was 1.65g/cm3Containing gas ofSoil slurry mass m required by soft soil triaxial soil sample3＝md2×2＝648.32g，
The dry density was 1.70g/cm3The soil slurry mass m required by the aerated soft soil triaxial soil sample4＝md3×2＝667.56g，
The density of the slurry prepared in this example is ρPulp and its production processIs 1.7545g/cm3By passing
Density formula, can calculate m2、m3And m4The required corresponding soil slurry volumes (two figures after decimal point calculation and reservation) are respectively as follows:
the dry density was 1.60g/cm3Volume V of soil slurry needed by aerated soft soil triaxial soil sample2＝358.10cm3＝358.10ml，
The dry density was 1.65g/cm3Volume V of soil slurry needed by aerated soft soil triaxial soil sample3＝369.52cm3＝369.52ml，
The dry density was 1.70g/cm3Volume V of soil slurry needed by aerated soft soil triaxial soil sample4＝380.48cm3＝380.48ml，
Thus, a dry density of 1.60g/cm was prepared3、1.65g/cm3And 1.70g/cm3The flow rates of the required soil slurry of the soil sample 210 are respectively as follows: 358.10ml, 369.52ml and 380.48 ml.
(4) The fifth valve 300 is opened to make the soil slurry in the soil sample reaction kettle 2 continuously flow into the soil sample forming box 3, and when the reading of the first flowmeter 208 is changed from 100ml to 358.10ml (or 369.52ml, 380.48ml), the fifth valve 300 is closed. Opening the eighth valve 305, slowly pushing the pushing piston 307 by using a jack, solidifying and compressing the soil slurry in the soil sample forming box 3 until the scale mark 306 on the pushing rod is 100mm (the height of the sample is 100mm), standing, and after the water head discharged into the high-pressure guide pipe B215 is stable and unchanged and exceeds 24 hours; closing the first valve 201, the fourth valve 207, the eighth valve 305; removing the conduits at the outer ends of the fifth valve 300 and the eighth valve 305; and (4) moving the soil sample forming box 3 into a freezing chamber for freezing and forming. After the forming, the mould of the soil sample forming box 3 is unscrewedThe bottom cover 304 pushes out the sample through the material pushing piston 307, and the soil sample 206 is quickly installed on the base of the triaxial apparatus; controlling the back pressure to be less than or equal to 200kPa by adopting a triaxial test system; after the soil sample 206 is melted, the water in the pores of the soil sample 206 slowly replaces the N in the zeolite powder 1042Qi until stable. Determining the pressure and N in the soil sample 206 from Henry's law based on the recorded volume, temperature and pressure2The relationship of air quantity, thus realizing the initial dry density of 1.60g/cm3(or 1.65 g/cm)3、1.70g/cm3) Preparing the gas-containing soil sample.
The invention prepares the aerated soft soil triaxial soil sample required by the geotechnical experiment of the embodiment (the experimental requirements are that the diameter d is 50mm, the height h is 100mm, and the volume V is2Is 196.34cm3Dry densities of 1.60, 1.65 and 1.70g/cm, respectively3) In addition, can also prepare the triaxial soil sample of the aerated soft soil of other geotechnical test requirement specifications, this embodiment only with preparation aerated soft soil triaxial soil sample (the experimental requirement is: diameter d of 50mm, height h of 100mm, volume V2Is 196.34cm3Dry densities of 1.60, 1.65 and 1.70g/cm, respectively3) The preparation process of the present invention is illustrated by way of example.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (8)
1. A variable density gas-containing soil sample preparation facilities based on zeolite replacement reaction which characterized in that: the device comprises a zeolite reaction kettle (1), a soil sample reaction kettle (2) and a soil sample forming box (3), wherein the bottom of the zeolite reaction kettle (1) is communicated with the middle part of the soil sample reaction kettle (2) through a high-pressure conduit A (107), the top of the zeolite reaction kettle (1) is communicated with an air inlet pipe B (108) and a first vacuum pressure gauge (101), and a first valve (100) is arranged on the air inlet pipe B (108); the top of the soil sample reaction kettle (2) is communicated with the bottom of the soil sample forming box (3) through a high-pressure guide pipe B (215), a third valve (201) is arranged at the position, close to the top of the soil sample reaction kettle (2), of the high-pressure guide pipe B (215), and an eighth valve (305) is arranged at the position, close to the bottom of the soil sample forming box (3), of the high-pressure guide pipe B (215); a stirrer (204) is correspondingly installed in the soil sample reaction kettle (2), the top of the soil sample reaction kettle (2) is communicated with an air inlet pipe A (211) and a second vacuum pressure gauge (209), a fifth valve (210) is arranged on the air inlet pipe A (211), and a thermometer (200) is arranged in the soil sample reaction kettle (2); the bottom of the soil sample reaction kettle (2) is communicated with a water inlet pipe (213), and a second flowmeter (212) and a sixth valve (214) are correspondingly arranged on the water inlet pipe (213); the bottom of the soil sample reaction kettle (2) is communicated with the top of the soil sample forming box (3) through a soil slurry communicating pipe (4), and the soil slurry communicating pipe (4) is sequentially provided with a fourth valve (207), a first flowmeter (208) and a seventh valve (300) from top to bottom; soil sample shaping box (3) bottom intercommunication is equipped with third vacuum pressure table (308), soil sample shaping box (3) are including mould top cap (301), moulded die (302) and mould bottom (304), the detachable seal installation in moulded die (302) top of mould top cap (301), the detachable seal installation in moulded die (302) bottom of mould bottom (304), mould top cap (301) are equipped with the material piston (307) that pushes away of taking the scale.
2. The apparatus for preparing a gas-containing soil sample with variable density based on zeolite substitution reaction according to claim 1, wherein: the zeolite reaction kettle (1) comprises a tank body (105) and a zeolite sealing cover (102) hermetically covering a tank opening at the top of the tank body (105), and the zeolite sealing cover (102) is fixedly connected with the top of the tank body (105) through a plurality of first bolts (103); the bottom of the tank body (105) is in a funnel shape, a second valve (106) is arranged at the position, close to the bottom of the tank body (105), of the high-pressure conduit A (107), and the air inlet pipe B (108) and the first vacuum pressure gauge (101) are respectively communicated and arranged on the zeolite sealing cover (102).
3. The apparatus for preparing a gas-containing soil sample with variable density based on zeolite substitution reaction according to claim 1, wherein: the material pushing piston (307) comprises a material pushing rod, a material pushing handle and a material pushing piston plate, the material pushing rod is installed on the die top cover (301) in a penetrating mode, the material pushing handle is fixed to the top end of the material pushing rod, the material pushing piston plate is fixed to the bottom end of the material pushing rod, the material pushing piston plate is located inside the forming die (302) in a matched mode, the material pushing handle is located outside the soil sample forming box (3), and the material pushing rod is provided with scale marks (306) in the height direction.
4. The apparatus for preparing a gas-containing soil sample with variable density based on zeolite substitution reaction according to claim 1, wherein: the soil sample reaction kettle (2) comprises a cylinder body (205) and a soil sample sealing cover (203) which is hermetically covered on a cylinder opening at the top of the cylinder body (205), and the soil sample sealing cover (203) and the top of the cylinder body (205) are further fixedly connected through a plurality of second bolts (202); the air inlet pipe A (211) and the second vacuum pressure gauge (209) are respectively communicated with and arranged on the soil sample sealing cover (203), and the end part of the high-pressure guide pipe B (215) is communicated and arranged on the soil sample sealing cover (203).
5. The apparatus for preparing a gas-containing soil sample with variable density based on zeolite substitution reaction according to claim 1, wherein: also comprises a vacuum pump and N2The vacuum pump is provided with an evacuation pipe, the evacuation pipe of the vacuum pump corresponds to the air inlet pipe A (211) and the air inlet pipe B (108) respectively, and N is2The storage tank is provided with an air outlet pipe, N2The air outlet pipe of the storage tank corresponds to the air inlet pipe A (211) and the air inlet pipe B (108) respectively.
6. The apparatus for preparing a gas-containing soil sample with variable density based on zeolite substitution reaction according to claim 4, wherein: agitator (204) include agitator motor, (mixing) shaft and stirring rake, the (mixing) shaft rotates to run through to be installed on the sealed lid of soil sample (203), a plurality of stirring rake is installed in the cooperation on the (mixing) shaft, and all stirring rakes all are located inside barrel (205), agitator motor installs on the sealed lid of soil sample (203), agitator motor's power output shaft and (mixing) shaft power are connected.
7. The apparatus for preparing a gas-containing soil sample with variable density based on zeolite substitution reaction according to claim 1, wherein: the end part of the high-pressure conduit B (215) is communicated and arranged on the die bottom cover (304), the bottom end of the slurry communicating pipe (4) is communicated and arranged on the die top cover (301), and the third vacuum pressure gauge (308) is communicated and arranged at the bottom of the forming die (302).
8. A preparation method of a variable-density gas-containing soil sample based on zeolite displacement reaction is characterized by comprising the following steps: the method comprises the following steps:
A. placing saturated permeable stone (309) and filter paper (303) on the mold bottom cover (304) in sequence, sealing the forming mold (302) through the mold top cover (301) and the mold bottom cover (304) to form a closed soil sample forming box (3), and weighing the total mass m of the soil sample forming box (3) at the moment0(ii) a Installing a soil sample reaction kettle (2) with mass m1The dried soil is put into a cylinder body (205), and a soil sample sealing cover (203) is closed; installing a zeolite reaction kettle (1) with mass m1The dried zeolite powder (104) is put into a zeolite reaction kettle (1), and a zeolite sealing cover (102) is closed;
B. the zeolite reaction kettle (1) is communicated with the soil sample reaction kettle (2) through a high-pressure guide pipe A (107), the soil sample reaction kettle (2) is communicated with the soil sample forming box (3) through a high-pressure guide pipe B (215), a vacuumizing pipe of a vacuum pump is hermetically communicated with an air inlet pipe A (211) and an air inlet pipe B (108) respectively, a fourth valve (207) and a sixth valve (214) are closed, a first valve (100), a third valve (201), a fifth valve (210), a seventh valve (300) and an eighth valve (305) are opened, and the vacuum pump is started to completely pump air in the zeolite reaction kettle (1), the soil sample reaction kettle (2) and the soil sample forming box (3); when the first vacuum pressure gauge (101), the second vacuum pressure gauge (209) and the third vacuum pressure gauge (308) are close to-100 kPa, continuing pumping air for not less than 1.5 hours, and then closing the first valve (100) and the fifth valve (210);
C. the air inlet pipe A (211) and the air inlet pipe B (108) are respectively connected with high-purity N2Storage tank, adjusting N2A pressure reducing valve of the storage tank to maintain the pressure at 300 kPa; opening the first valve (100) and the fifth valve (210), and closing the first valve (100) and the fifth valve (210) after the first vacuum pressure gauge (101) and the second vacuum pressure gauge (209) are stabilized at 300 kPa;
D. opening a second valve (106) to enable zeolite powder (104) in the tank body (105) to fall into the soil sample reaction kettle (2), then closing the second valve (106) and opening a stirrer (204) for stirring operation to enable dried soil and zeolite powder (104) to be uniformly mixed, and recording the temperature value of the thermometer (200);
E. immersing the inlet pipe (213) in the distilled water in the water tank, opening the sixth valve (214) to allow the distilled water to be slowly injected into the cylinder (205) through the inlet pipe (213), and recording the flow reading V on the second flow meter (212)0Closing the sixth valve (214); turning on the stirrer (204) for stirring to uniformly mix the soil and the water to form soil slurry;
F. opening a fourth valve (207) and a seventh valve (300), allowing the soil slurry in the soil sample reaction kettle (2) to flow into the soil sample forming box (3) under the action of gravity, recording the flow through a first flow meter (208), and closing the seventh valve (300) after the required soil slurry flows into the soil sample forming box (3);
G. opening an eighth valve (305), and slowly pushing a material pushing piston (307) by using a jack to solidify and deform the soil slurry until the sample height of the required soil sample (206) is reached; the eighth valve (305) is closed after standing and the waterhead to be discharged into the high-pressure conduit B (215) is stable and exceeds 24 hours; removing the soil slurry communicating pipe (4) and the high-pressure guide pipe B (215), and integrally moving the soil sample forming box (3) into a freezing chamber for freezing and forming; after the forming, the mould bottom cover (304) of the soil sample forming box (3) is unscrewed, the soil sample (206) is pushed out through the material pushing piston (307),rapidly mounting a soil sample (206) on a base of the triaxial apparatus; controlling the back pressure to be less than or equal to 200kPa by a triaxial test system, and gradually and slowly replacing N adsorbed in the zeolite powder (104) by water in pores of the soil sample (206) after the soil sample (206) is melted2Qi until stable.
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