CN112729992A - Thermophysical property testing device for organic contaminated soil - Google Patents

Thermophysical property testing device for organic contaminated soil Download PDF

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Publication number
CN112729992A
CN112729992A CN202110069999.5A CN202110069999A CN112729992A CN 112729992 A CN112729992 A CN 112729992A CN 202110069999 A CN202110069999 A CN 202110069999A CN 112729992 A CN112729992 A CN 112729992A
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China
Prior art keywords
sample
soil
sample cylinder
cylinder
testing
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Pending
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CN202110069999.5A
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Chinese (zh)
Inventor
范利武
吴宇豪
徐馨宇
胡楠
俞自涛
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Zhejiang University ZJU
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Zhejiang University ZJU
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Priority to CN202110069999.5A priority Critical patent/CN112729992A/en
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/286Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N25/00Investigating or analyzing materials by the use of thermal means
    • G01N25/20Investigating or analyzing materials by the use of thermal means by investigating the development of heat, i.e. calorimetry, e.g. by measuring specific heat, by measuring thermal conductivity

Abstract

The invention relates to a thermophysical property testing device for organic contaminated soil, and the testing principle is based on a double-probe method. The device adopts the density of piston compaction's mode control soil sample, the position of the fixed slider that embeds two probes of structure of design screw hole and countersunk screw makes the sample section of thick bamboo airtight in order to prevent organic pollutant and the moisture loss in the soil sample, select for use and can tolerate 500 ℃ of high temperature material as sample section of thick bamboo, sample section of thick bamboo lid, slider guide cylinder, slider, probe inside insulation heat conduction filler and thermocouple, the material of wire cluster outer cladding layer, can effectively test the thermal conductivity of organic contaminated soil in-20 ~ 500 ℃ of scope, thermal diffusivity and specific heat capacity.

Description

Thermophysical property testing device for organic contaminated soil
Technical Field
The invention relates to a soil thermophysical property testing device, in particular to a wide-temperature-zone thermophysical property testing device for organic contaminated soil, and belongs to the field of engineering thermophysics, environmental science and engineering.
Background
In recent years, most of the seriously polluted enterprises once located in cities have stopped production, rectified or moved to suburbs, and more industrial polluted sites are left. To ensure safety, the soil in these contaminated sites must be remediated before reuse. The thermal desorption technology is a repairing technology suitable for organic contaminated soil, and various organic pollutants in the soil are volatilized and removed by heating and increasing the temperature of the soil. At present, the maximum temperature of thermal desorption can reach more than 500 ℃, and exceeds the boiling point of most polycyclic aromatic hydrocarbons. Heating the soil to such high temperatures consumes a large amount of energy, so the cost of the current technology is as high as about 5000 yuan/m3. If a large number of soil thermophysical parameters under different conditions of temperature, density, water content, organic pollutant types, concentration and the like can be measured, the heat transfer characteristics of soil and the temperature distribution rule of a field in the thermal desorption process can be mastered, and then the accuracy of energy consumption prediction can be improved and a method for reducing the energy consumption can be searched.
None of the commercial instruments currently used for thermophysical testing meet the above requirements: the thermal physical property analyzer of KD2 Pro and TEMPOS based on the thermal probe method is simple and convenient to operate, but is only applicable to the temperature range of-50-150 ℃; although the Discovery xenon lamp heat conduction instrument based on the laser flash method can reach the high temperature of more than 500 ℃, a sample chamber needs to be vacuumized, and original water and organic pollutants in soil cannot be reserved, so that the test result cannot reflect the influence of the water content, the pollutant types and the concentration on the soil thermophysical property.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a thermophysical property testing device for organic contaminated soil, which can effectively test the thermal conductivity, thermal diffusivity and specific heat capacity of the organic contaminated soil under the conditions of accurately controlling the density of a sample and preventing the escape of water and pollutants; the wide temperature range is from-20 ℃ under the working condition of frozen soil to 500 ℃ above the boiling point of polycyclic aromatic hydrocarbon.
In order to achieve the purpose, the invention adopts the following technical scheme:
the thermophysical property testing device for the organic contaminated soil is characterized by comprising a host, a thermostat and a sample cylinder arranged in the thermostat, wherein a soil sample is filled in the sample cylinder; a sample cylinder cover is arranged at the top of the sample cylinder, and an air suction hole is formed in the side surface of the sample cylinder; the test sample cylinder cover is connected with the test sample cylinder through a test sample cylinder top thread, a slide block guide cylinder is fixed at the top of the test sample cylinder cover, a slide block is arranged in the slide block guide cylinder, the lower part of the slide block is connected with a probe, and a hole for enabling the probe to extend into the test sample cylinder is formed in the test sample cylinder cover; when the bottom end of the sliding block is contacted with the sample cylinder cover, the sliding block is fixed by screwing a countersunk screw into a threaded hole of the wall of the sliding block guide cylinder on the side surface of the sliding block guide cylinder;
the host comprises a direct current power supply, a temperature collector and a microcomputer; the host is connected with the probe through a wire, and a test hole for the wire to pass through is formed in the constant temperature box;
the probe comprises a stainless steel pipe, and an insulating heat-conducting filler, a heating wire and a thermocouple which are arranged in the stainless steel pipe; the temperature measuring point of the thermocouple is welded on the inner wall of the stainless steel pipe, and the electric heating wire is connected with a direct current power supply through a lead; the thermocouple is connected with a temperature collector through a wire, and the temperature collector is connected with a microcomputer.
In the technical scheme, further, before the soil sample in the sample cylinder is tested, a soil sample compaction device is adopted to compact the soil test; the soil sample compaction device is as follows: the top of the sample cylinder is connected with a piston guide cylinder through threads, a piston is arranged in the piston guide cylinder, and the piston is used for compacting the soil sample, so that the upper end face of the soil sample is flush with the upper end face of the threads on the top of the sample cylinder.
The material capable of resisting high temperature of 500 ℃ is selected as the material of the sample cylinder, the sample cylinder cover, the slide block guide cylinder, the slide block, the insulating heat-conducting filler in the probe, the thermocouple and the outer cladding layer of the wire cluster, and the thermal conductivity, the thermal diffusivity and the specific heat capacity of the organic contaminated soil can be effectively tested within the range of-20-500 ℃.
The device of the invention has the advantages that:
according to the thermophysical property testing device for the organic contaminated soil, disclosed by the invention, the testing principle is based on a double-probe method, the density of a soil sample is controlled in a piston compaction mode, various materials capable of resisting the high temperature of 500 ℃ are selected as materials of key parts such as a sample cylinder, a probe, a wire cluster and the like, the positions of the probe are fixed by designing structures of a threaded hole and a countersunk screw, so that the sample cylinder is sealed to prevent the organic contaminants and water in the soil sample from escaping, the defects that the temperature range of the existing testing technology is small, the organic contaminants and water cannot be prevented from escaping in the heating process and the like are overcome, the thermal conductivity, the thermal diffusivity and the specific heat capacity of the organic contaminated soil can be tested in the range of-20-500 ℃, and the testing result can provide a basis for energy consumption calculation.
Drawings
FIG. 1 is a schematic view of a soil sample compaction device connection;
FIG. 2 is a schematic connection diagram of a soil sample thermophysical property testing device;
FIG. 3 is a schematic diagram of the internal structure and connections of the probe and the host;
in the figure: 1, soil sample; 2, a sample cylinder; 3, air exhaust holes; 4, sample cylinder top threads; 5, a piston guide cylinder; 6, a piston; 7, a sample cylinder cover; 8, a slide block guide cylinder; 9, a sliding block; 10, a probe; 11 a slide block guide cylinder wall threaded hole; 12, countersunk head screws; 13 a thermostat; 14 test wells; 15 wire clusters; 16 host computer; 17 stainless steel tubes; 18 an insulating thermally conductive filler; 19 heating wires; 20 thermocouples; 21 a direct current power supply; 22 a temperature collector; 23 a microcomputer.
Detailed Description
Referring to fig. 1 to 3, a device for testing thermophysical properties of organic contaminated soil is described in detail below with reference to the accompanying drawings.
The device for testing the thermophysical properties of the organic contaminated soil comprises a soil sample 1, a sample cylinder 2, sample cylinder top threads 4, a piston guide cylinder 5, a piston 6, a sample cylinder cover 7, a slide block guide cylinder 8, a slide block 9, a probe 10, slide block guide cylinder wall threaded holes 11, countersunk screws 12, a constant temperature box 13, a wire cluster 15, a host computer 16, a direct current power supply 21, a temperature collector 22 and a microcomputer 23. The side wall of the sample cylinder 2 is provided with an air suction hole 3, the sample cylinder 2 is connected with a piston guide cylinder 5 or a sample cylinder cover 7 through a sample cylinder top thread 4, the slider guide cylinder 8 is welded at the upper end of the sample cylinder cover 7, the slider 9 can move up and down in the slider guide cylinder 8 and is internally welded with two identical probes 10, a slider guide cylinder wall thread hole 11 is used for screwing a countersunk screw 12 so that the bottom of the slider 9 is tightly attached to the sample cylinder cover 7, and the sample cylinder cover 7 is provided with a hole which has the diameter and the position which are just used for inserting the probes 10. The probe 10 comprises a stainless steel tube 17, and an insulating heat-conducting filler 18, a heating wire 19 and a thermocouple 20 which are arranged in the stainless steel tube 17. The temperature measuring point of the thermocouple 20 is welded on the inner wall of the stainless steel pipe 17, the top or the side wall of the constant temperature box 13 is provided with a testing hole 14 for a wire cluster 15 to be connected into the box, the host computer 16 comprises a direct current power supply 21, a temperature collector 22 and a microcomputer 23, the electric heating wire 19 is connected with the direct current power supply 21 through a wire in the wire cluster 15, the thermocouple 20 is connected with the temperature collector 22 through a wire in the wire cluster 15, and the temperature collector 22 is connected with the microcomputer 23.
The soil sample 1 can be collected by an organic pollution site or prepared by a laboratory; the sample cylinder 2 is made of stainless steel and is used for containing a soil sample 1; the extraction hole 3 is positioned on the side wall of the sample cylinder 2, comprises a valve, is closed when the soil sample 1 is compacted and the thermophysical property is tested, is connected with a vacuum extraction device after the test is finished, opens the valve, extracts volatilized organic pollutants and performs centralized treatment; the sample cylinder top thread 4 is used for fastening the sample cylinder 2 and the piston guide cylinder 5 during sample preparation, and fastening the sample cylinder 2 and the sample cylinder cover 7 during test; the bottom end of the piston guide cylinder 5 is provided with an internal thread; the piston 6 is matched with the piston guide cylinder 5 to compact the soil sample 1, so that the upper end surface of the soil sample 1 is flush with the upper end surface of the sample cylinder top thread 5, namely the soil sample 1 is filled in the whole sample cylinder 2; the sample cylinder cover 7 is made of stainless steel, contains internal threads and is provided with two round holes, and the positions and the diameters of the round holes are just suitable for the two probes 10 to be inserted; the slide block guide cylinder 8 is made of stainless steel and is welded at the upper end of the sample cylinder cover 7; the slide block 9 is made of stainless steel, two probes 10 are welded in the slide block 9, and the probes 10 are driven to move up and down in the slide block guide cylinder 8; the probe 10 comprises a stainless steel tube 17, an insulating heat-conducting filler 18, a heating wire 19 and a thermocouple 20, and when the probe 10 is completely inserted into the soil sample 1 through two small holes of the sample cylinder cover 7, the bottom end of the sliding block 9 is contacted with the top end of the sample cylinder cover 7; the slider guide cylinder wall threaded hole 11 is screwed in the countersunk screw 12 to fix the slider 9; the countersunk head screw 12 is screwed into the threaded hole 11 of the wall of the guide cylinder of the sliding block after the bottom end of the sliding block 9 is contacted with the top end of the sample cylinder cover 7, so that the sliding block 9 is prevented from being jacked open by the thermal expansion of the gas-phase substances in the soil sample 1 during testing; the constant temperature box 13 is used for controlling the temperature of the soil sample 1 to a certain set value, and the temperature control range meets the requirement of-20-500 ℃; the wire cluster 15 contains a plurality of insulated wires, and is coated by heat-insulating materials which can resist the high temperature of 500 ℃, such as calcium silicate, perlite, ceramic fiber and the like, and the probe 10 welded in the sliding block 9 is connected with the host 16; the front end of the stainless steel pipe 17 is of a conical structure, the inside of the pipe is of a hollow structure, and the ratio of the length to the diameter is not less than 50; the insulating heat-conducting filler 18 is made of materials capable of resisting high temperature of 500 ℃, such as corundum and mica, and is filled in the stainless steel pipe 17, and the positions of the electric heating wire 19 and the thermocouple 20 are fixed to ensure that the surface of the stainless steel pipe is electrically insulated; the electric heating wire 19 is connected with a direct current power supply 21 in the host 17 through a lead in the lead cluster 15 and is used as an internal heat source of the probe 10; the thermocouple 20 is made of a material capable of resisting the high temperature of 500 ℃, a K-type or E-type thermocouple is recommended to be used and is connected with a temperature collector 22 in the host 17 through a lead in the lead cluster 15, and a temperature measuring point is welded on the inner wall of the stainless steel pipe 17; the direct current power supply 21 provides adjustable direct current for the heating wire 19 in the probe 10, and has multi-channel output capability; the temperature collector 22 collects temperature data of the thermocouple 20 in the probe 10 and has multi-channel output capacity; and the microcomputer 23 is connected with the temperature collector 22, stores temperature data and calculates the thermal conductivity, thermal diffusivity and specific heat capacity of the soil.
The method comprises the following specific implementation steps:
section 1-specimen compaction: step 1, fastening a sample cylinder 2 and a piston guide cylinder 5, and closing a valve of an air suction hole 3; step 2, weighing a certain mass of soil sample 1, pouring the soil sample into a container consisting of a sample cylinder 2 and a piston guide cylinder 5, and pressing the upper end surface of the soil sample 1 to be flush with the upper end surface of a sample cylinder top thread 5 by using a piston 6; and step 3, pulling out the piston 6 to separate the sample cylinder 2 from the piston guide cylinder 5. The piston 6 compacts the soil sample 1 to fill the sample cylinder 2, and the volume V of the soil sample 1 is equal to the volume of the sample cylinder 2, so the mass m of the soil sample 1 to be weighed is calculated from the preset density ρ and the volume of the sample cylinder 2.
Part 2-test calculation: step 1, fastening a sample cylinder 2 and a sample cylinder cover 7 welded with a slide block guide cylinder 8, and placing the sample cylinder in a constant temperature box 13; step 2, the slide block 9 welded with the probe 10 is placed in a slide block guide cylinder 7, and a wire cluster 15 connected with the probe 10 is connected with a host 15 outside a constant temperature box 13 through a test hole 14; step 3, the slide block 9 is pressed downwards to move to the bottom of the slide block guide cylinder 8, namely the bottom of the slide block 9 is contacted with the top of the sample cylinder cover 7, and at the moment, the two probes 10 are completely inserted into the soil sample 1; step 4, screwing a countersunk screw 12 into the threaded hole 11 of the wall of the slide block guide cylinder to fix the position of the slide block 9, so that the effect of sealing the sample cylinder 2 is achieved; step 5, marking the two probes 10 as A and B respectively, fixing the distance r between the two probes, and reading the temperature T of the thermocouple 20 in the two probes 10AAnd TBNamely the temperature of the soil near the temperature measuring point; step 6, switching on a power supply of the constant temperature box, and setting a temperature value T required to be controlled0(ii) a Step 7, wait for TAAnd TBStabilized at T0After the proximity, constant current I was applied to probes A and B, respectivelyAAnd IBRecording time T from the application of current and recording at a certain frequencyAAnd TB(ii) a change in (c); step 8, according to r and IA、IBλ, τ and TACurve of (d), τ and TBThe thermal conductivity lambda and the thermal diffusivity a of the soil are calculated by the curve, and the specific heat capacity c of the soil is calculated by combining the density rho.
Part 3 — exhaust gas extraction: step 1, cutting off the power supply of the constant temperature box, opening the box door, and slightly cooling; and 2, connecting the vacuum extraction equipment with the extraction hole 3, opening a valve, and extracting and intensively treating the organic pollutants which are changed into gas phase.
The principle of measuring and calculating the thermal conductivity lambda, thermal diffusivity a and specific heat capacity c of a material by using the double probe method is well known to those skilled in the art and will not be described in detail in the present specification.

Claims (9)

1. The thermophysical property testing device for the organic contaminated soil is characterized by comprising a host, a thermostat and a sample cylinder arranged in the thermostat, wherein a soil sample is filled in the sample cylinder; a sample cylinder cover is arranged at the top of the sample cylinder, and an air suction hole is formed in the side surface of the sample cylinder; the test sample cylinder cover is connected with the test sample cylinder through a test sample cylinder top thread, a slide block guide cylinder is fixed at the top of the test sample cylinder cover, a slide block is arranged in the slide block guide cylinder, the lower part of the slide block is connected with a probe, and a hole for enabling the probe to extend into the test sample cylinder is formed in the test sample cylinder cover; when the bottom end of the sliding block is contacted with the sample cylinder cover, the sliding block is fixed by screwing a countersunk screw into a threaded hole of the wall of the sliding block guide cylinder on the side surface of the sliding block guide cylinder;
the host comprises a direct current power supply, a temperature collector and a microcomputer; the host is connected with the probe through a wire, and a test hole for the wire to pass through is formed in the constant temperature box;
the probe comprises a stainless steel pipe, and an insulating heat-conducting filler, a heating wire and a thermocouple which are arranged in the stainless steel pipe; the temperature measuring point of the thermocouple is welded on the inner wall of the stainless steel pipe, and the electric heating wire is connected with a direct current power supply through a lead; the thermocouple is connected with a temperature collector through a wire, and the temperature collector is connected with a microcomputer.
2. The apparatus for testing the thermophysical properties of organic contaminated soil according to claim 1, wherein the sample cylinder, the sample cylinder cover, the slide guide cylinder and the slide are made of stainless steel.
3. The apparatus for testing the thermal physical properties of the organically-polluted soil according to claim 1, wherein the suction hole is provided with a valve which is closed when the soil sample is compacted and tested and opened after the test is completed and the vacuum extraction device is connected to extract the organic pollutants which have been converted into the gas phase.
4. The apparatus for testing the thermophysical properties of the organically-polluted soil according to claim 1, wherein two of the probes are identical and have a length to diameter ratio of not less than 50.
5. The apparatus for testing the thermophysical properties of the organically-polluted soil as claimed in claim 1, wherein the insulating and heat-conducting filler and the thermocouple are made of materials capable of withstanding a high temperature of 500 ℃.
6. The apparatus for testing the thermophysical properties of the organically-polluted soil according to claim 1, wherein the lead is provided in a cluster of leads, and the cluster of leads is covered with a heat insulating material capable of withstanding a high temperature of 500 ℃.
7. The apparatus for testing the thermophysical properties of the organically-polluted soil according to claim 1, wherein the temperature of the incubator is controlled within a range of-20 ℃ to 500 ℃.
8. The device for testing the thermophysical properties of the organic contaminated soil according to claim 1, wherein the direct-current power supply and the temperature collector both have multi-channel output capability.
9. The apparatus for testing the thermophysical properties of the organically-polluted soil according to claim 1, wherein the soil sample in the sample cylinder is compacted by a soil sample compacting apparatus before the test; the soil sample compaction device is as follows: the top of the sample cylinder is connected with a piston guide cylinder through threads, a piston is arranged in the piston guide cylinder, and the piston is used for compacting the soil sample, so that the upper end face of the soil sample is flush with the upper end face of the threads on the top of the sample cylinder.
CN202110069999.5A 2021-01-19 2021-01-19 Thermophysical property testing device for organic contaminated soil Pending CN112729992A (en)

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Application publication date: 20210430