CN111999156A - Temperature-controlled high-pressure biological solidification test device and test method thereof - Google Patents
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- 230000008023 solidification Effects 0.000 title claims abstract description 33
- 238000012360 testing method Methods 0.000 title claims abstract description 30
- 238000010998 test method Methods 0.000 title abstract description 5
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- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims description 6
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- 239000004202 carbamide Substances 0.000 claims description 4
- VSGNNIFQASZAOI-UHFFFAOYSA-L calcium acetate Chemical compound [Ca+2].CC([O-])=O.CC([O-])=O VSGNNIFQASZAOI-UHFFFAOYSA-L 0.000 claims description 3
- 239000001639 calcium acetate Substances 0.000 claims description 3
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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
- G01N1/44—Sample treatment involving radiation, e.g. heat
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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
- G01N2001/366—Moulds; Demoulding
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Abstract
The invention discloses a temperature-controlled high-pressure biological solidification test device and a test method thereof, wherein the device provides high-pressure confining pressure for a sample by utilizing a pressure chamber air inlet pipe, a pressure chamber sealing cover and a pressure chamber; the sample penetration length was controlled using a sample cap and control bolt. A control by temperature change heating device has been installed under the base for place the sample for temperature constancy in the sample curing process. Under the conditions of constant temperature and high pressure, a biochemical perfusate is injected into a control end and a biochemical perfusate outlet end, a solution for solidification is perfused into a sample for solidification, wherein the solidified sample is wrapped by a rubber membrane. The device can be used for simulating the solidification process of biological induction calcium carbonate under the high-pressure condition, exploring the filling effect of biomineralization filling ore body goaf under different temperatures and high-pressure conditions after underground ore body mining, and providing guarantee for the integrity and stability of the mined-out stratum structure.
Description
Technical Field
Although biological species play an indispensable role in the earth formation process, human beings do not have much understanding about the mechanism of action and the relationship with the environment of biological species in the earth formation process. The invention relates to a biological curing device, in particular to a temperature-control high-pressure biological curing device and a test method thereof, which are mainly used for a biological strain mineralization mechanism under high pressure.
Background
China develops rapidly in recent years and has great demand on underground mineral resources. With continuous exploitation of underground minerals such as petroleum and combustible ice, pores are left in the stratum, which can cause engineering diseases such as stratum settlement, collapse, instability and the like, and cause great potential safety hazard and economic loss. Therefore, biochemical solution is injected into the mined-out area of the underground ore body by adopting a microbial mineralization technology, and calcium carbonate is formed to fill the pores left after the petroleum or combustible ice is mined, so that the stability of the stratum is improved. However, underground ore body filling involves different temperature and high pressure environments, which brings great difficulties to engineering implementation.
Biogenetic mineralization is a natural phenomenon that plays an important role in the history of earth formation, which is the result of recent thirty years of geochemical research. Recognizing the action and position of biological diagenesis and mineralization again, has important significance for the technical development of geotechnical engineering. The principle is that urea is continuously decomposed by urease to form CO3 2-Ca in negatively charged aqueous solution and in environment of continuously chelating organic matter2+Inducing local crystal anions (CO)3 2-) With CO3 2-The concentration is further increased to attract more Ca2+Up to the crystal surface CaCO3The concentration is increased to be continuously nucleated, and CaCO is finally deposited3And (3) granules. In recent years, the technology has attracted much attention in the fields of rock and soil and materials, and the technology is often used for solidifying sandy soil.
For the research of related test devices, for example, patent application publication No. CN109959773A discloses a test device and method for reinforcing silt by slip casting of microorganisms, which is composed of GDS pressure controller, slurry storage device, reaction device and filtrate collection bottle 4. The GDS pressure controller provides pressure to accurately control the grouting speed, so that the slurry is slowly and uniformly injected into the soil sample. The sample preparation barrel in the reaction device is formed by butting two organic glass tubes, so that the sealing property of the device can be ensured, and the complete demoulding can be facilitated. The silt is solidified by utilizing the microbial mineralization technology, and the method of injecting the bacterial liquid and the cementing liquid step by step is adopted, so that the blockage of a grouting opening caused by the direct mixing of the cementing liquid and the bacterial liquid is better avoided. And meanwhile, the mode of up-up grouting from bottom is adopted, so that grouting liquid can be better uniformly distributed in the soil sample, and the uniformity and integrity of soil sample solidification are ensured.
Patent application document with publication number CN109540630A discloses a combined sample preparation device and method for reinforcing sandy soil in batches by microorganisms, and belongs to the field of calcareous sand foundation reinforcement. The device comprises a cementing curing box, wherein the cementing curing box is provided with an interlayer water tank, and a temperature-controllable heater and a circulating water pump are arranged in the interlayer water tank; the sand filling mold assembly arranged in the cementing curing box comprises a soft plastic pipe, wherein gauze is wound on the outer wall of the soft plastic pipe, and the upper and lower openings and the side wall of the soft plastic pipe are provided with air holes; and the filter paper and the permeable stone sequentially cover the upper opening and the lower opening of the soft plastic pipe. The method provided by the invention utilizes the mineralization of the microbial liquid to bond the sand, effectively reinforces the sand through a set of designed solidification sample preparation device, is simple and feasible, and is easy for batch production of the microbial solidification cylindrical sandy soil test piece for related tests. The sample preparation device and the sample preparation method greatly improve the sample preparation efficiency and the uniformity of the cemented sample, also obviously reduce the difference between different samples and meet the test repeatability and the multi-sample requirements.
Chinese patent CN201610828703.2 discloses a method for preparing calcium carbonate solidified sandy soil by using microorganisms, sand is poured into a bottle to uniformly cover the bottom of the bottle, then a gelling liquid and a cultured bacterial liquid are poured, shaking culture is carried out at a constant temperature, then a part of mixed liquid in the bottle is quantitatively absorbed every day, an equal amount of gelling liquid is added, a small amount of sand is uniformly added, and finally, a solidified sand column is obtained after lasting for several days; however, this method usually requires a lot of manpower and material resources and is not suitable for the environment with high temperature and pressure.
Disclosure of Invention
The purpose of the invention is as follows: the inventor provides a temperature-control high-pressure biological solidification device and a test method thereof on the basis of a previously applied patent (CN 201610828703.2, hereinafter referred to as patent 1) for simulating the filling effect of biomineralization filling of a mined-out area of an ore body under different temperature and high pressure conditions after mining of an underground ore body, wherein the biomineralization filling of the mined-out area of the ore body is facilitated when the temperature is lower than 80 ℃ and the pressure is increased to form calcium carbonate, and when the seepage speed is too high and the fire is too low, the biomineralization is not facilitated to form calcium carbonate. Has the functions of controlling temperature, providing high pressure environment and carrying out biological solidification.
The technical scheme is as follows: in order to realize the purpose of the invention, the invention adopts the following technical scheme:
the biochemical perfusate (solidification liquid) mentioned below in the invention is described in patent 1 and consists of a bacterial liquid, a calcium chloride solution and a gelling liquid. The gel liquid is 0.5mol/L calcium acetate and each liter of the solution is dissolved by adding 30g of urea to obtain a mixed solution, the bacterial liquid is bacillus pasteurii, and the OD600 value is 2.268. The concentration of the calcium chloride solution is 0.05mol/L, and the ratio of the calcium chloride solution, the bacterial liquid and the gel liquid is 1: 5: 10.
Because of the different curing liquids used, the solutions described in the background art are not suitable.
The utility model provides a biological solidification technology device under control by temperature change high pressure, is including the base that is used for placing the sample, is equipped with the pressure chamber on the base, and the pressure chamber outside is equipped with the sealed cowling, and the pressure chamber is connected pressure chamber discharge valve and intake pipe.
The high-pressure confining pressure is provided for the sample by injecting water into the pressure chamber, and the pressure in the test process is measured in real time by utilizing a pressure gauge on the air inlet pipe.
In order to prevent the deformation of the specimen, a specimen cap and a control bolt are loaded on the top of the specimen, and the specimen length (i.e., height, permeation path) is controlled using the specimen cap and the control bolt.
A temperature control heating device is arranged under the base, so that the temperature constancy in the sample curing process is ensured. Wherein the surface of the cured sample is wrapped with a rubber film.
The test process of the biological solidification technology device under the temperature control high pressure comprises the following steps:
1) preparing a sample to be cured according to the required initial density, sleeving a rubber film on the sample to be cured, fixing the rubber film on a base, and covering a sample cap on the top of the sample.
2) And a sealing cover is sleeved on the outer side of the pressure chamber, the bolt is fastened, the sealing and air-tightness of the pressure chamber are ensured, and the length of the control sample, namely the penetration length, of the control bolt 7 is reduced.
3) Closing pressure chamber discharge valve, utilizing the intake pipe injection gas, providing the confining pressure of high pressure for the sample, when injecting gas, the real-time observation manometer controls pressure (confining pressure) in the testing process, closes the intake pipe after reaching the pressure of needs.
4) And opening the temperature control heating device under the base, and adjusting to ensure that the temperature is constant in the test process.
5) And the biochemical perfusate is injected into the control end, the solidified liquid required by solidification is perfused into the sample from the bottom, and the solidified liquid flows out through the outlet end of the biochemical perfusate. After the perfusion is finished, the biochemical perfusate injection and control end and the biochemical perfusate outlet end are closed simultaneously.
6) And 5) repeatedly circulating the pouring step for many times so as to achieve the required curing strength.
The technical effects are as follows: the temperature-controlled high-pressure biological solidification device provided by the invention can simulate different temperature and high-pressure conditions to ensure that a sample can be solidified and molded by using a biological mineralization technology under different constant temperature and high pressure conditions, so that the filling effect of filling the goaf of the underground ore body by using a biological technology after the underground ore body is mined in a solidification effect research project can be realized, the strength of the mined underground ore body is improved, and the damage of settlement and collapse is prevented.
Drawings
FIG. 1 is a schematic view of a biological solidification apparatus under temperature-controlled high pressure.
Wherein: a pressure chamber exhaust valve-1, a sealing cover-2, a pressure chamber-3, a sample-4, a rubber membrane-5, a sample cap-6, a control bolt-7, a biochemical perfusate outlet end-8, a pressure gauge-9, an air inlet pipe-10, a base-11, a biochemical perfusate injection and control end-12 and a temperature control heating device-13.
Detailed Description
The technical solution of the present invention will be specifically described below with reference to examples:
referring to fig. 1, a biological solidification technology device under control by temperature change high pressure, including the base 11 that is used for placing the sample, be equipped with pressure chamber 3 on the base, the pressure chamber 3 outside is equipped with sealed cowling 2, prevents gas leakage through setting up sealed cowling 2 and pressure chamber 3, pressure chamber 3 is connected pressure chamber discharge valve 1 and intake pipe 10, provides the confining pressure of high pressure for sample 4 through injecting gas to utilize manometer 9 on the intake pipe 10 to carry out real-time measurement to the pressure in the test process.
In order to prevent the deformation of the sample, a sample cap 6 and a control bolt 7 are loaded on the top of the sample, and axial pressure is provided to the sample by the sample cap 6 and the control bolt 7. A temperature control heating device 13 is arranged below the base 11, so that the temperature is constant in the sample curing process. Under the conditions of constant temperature and high pressure, a biochemical perfusion solution is injected into the control end 12 and the biochemical perfusion solution outlet end 8, the biochemical perfusion solution for solidification is perfused into a sample from the bottom, the sample is output from the top, and the sample is solidified, wherein the surface of the solidified sample is wrapped by the rubber membrane 5.
The test process of the biological solidification technology device under the temperature control high pressure comprises the following steps:
1) preparing a sample (rock sample) to be cured according to the required initial density, sleeving a rubber membrane 5, fixing the rubber membrane on a base 11, and covering a sample cap 6 on the top of the sample.
2) The sealing cover 2 is sleeved on the outer side of the pressure chamber 3, the bolt is fastened, the pressure chamber 3 is sealed and airtight, and the length of the control sample, namely the penetration length, of the control bolt 7 is reduced.
3) Closing pressure chamber discharge valve 1, utilizing intake pipe 10 to inject into gas, providing the confining pressure of high pressure for sample 4, when injecting into gas, real-time observation manometer 9, pressure (confining pressure) among the control test process closes intake pipe 10 after reaching the pressure of needs.
4) The temperature control heating device 13 under the base 11 is opened, and the temperature is constant in the test process through adjustment
5) And the biochemical perfusate is injected into the control end 12, the solidification liquid required by solidification is perfused into the sample from the bottom, and the solidification liquid flows out through the biochemical perfusate outlet end 8. After the perfusion is finished, the biochemical perfusate injection and control end 12 and the biochemical perfusate outlet end 8 are closed at the same time.
6) And 5) repeatedly circulating the pouring step for many times so as to achieve the required curing strength.
Examples 1-5 are the effects of curing the samples at different ambient pressures and temperatures, and the conditions and results are shown in Table 1.
TABLE 1
TABLE 2
In the process of oil field exploitation, water injection and oil displacement are performed, but under the condition that the pore connectivity of an oil storage layer of an old oil field (such as Daqing and Shengli oil fields) is good, more water is injected and oil is displaced. Therefore, the device is used for researching solidification tests with different pressures and different perfusion speeds under the temperature control condition and is combined with CT analysis to research the pore-throat effect of organisms. The invention injects air into the pressure chamber, applies different pressures to the sample (1), and implements temperature control (2) and adjusts the perfusion speed (3) through the temperature control heating device below the base; from the effect of the test, the best effect can be achieved only under the appropriate pressure, perfusion speed and temperature aiming at the selected sample/rock sample, and particularly, the hardness of the sample after solidification can reach 1.0-8.0 MPa at the temperature of 45-70 ℃, the confining pressure of 1.0-10.0MPa and the perfusion speed of 1.0-4.0 mL/min.
The above description is only of the preferred embodiments of the present invention, and it should be noted that: it will be apparent to those skilled in the art that various modifications and adaptations can be made without departing from the principles of the invention and these are intended to be within the scope of the invention.
Claims (5)
1. A biological solidification test device under temperature control and high pressure is characterized by comprising a base for placing a sample, wherein a pressure chamber is arranged on the base, a sealing cover is arranged outside the pressure chamber, and the pressure chamber is connected with an exhaust valve and an air inlet pipe of the pressure chamber; a temperature control heating device is arranged under the base; and a sample cap and a control bolt are loaded on the top of the sample, and the length of the controllable sample is adjusted by using the sample cap and the control bolt.
2. The testing method of the biological solidification testing device under the temperature-controlled high pressure as claimed in claim 1, characterized by comprising the following steps:
1) preparing a sample to be solidified according to the required initial porosity, fixing the sample on a base, and covering a sample cap on the top of the sample;
2) sleeving a sealing cover on the outer side of the pressure chamber, fastening the bolt, ensuring that the pressure chamber is sealed and airtight, and reducing the length of the control bolt for controlling the sample;
3) closing an exhaust valve of the pressure chamber, injecting gas by using an air inlet pipe, providing high-pressure confining pressure for a sample, observing a pressure gauge in real time while injecting the gas, controlling the pressure in the test process, and closing the air inlet pipe after the required pressure is reached;
4) opening a temperature control heating device below the base, and adjusting to ensure that the temperature is constant in the test process;
5) injecting a solidification liquid required for solidification into the sample from the bottom by using a biochemical perfusion liquid injection and control end, and allowing the solidification liquid to flow out through a biochemical perfusion liquid outlet end; after the perfusion is finished, closing the biochemical perfusate injection and control end and the biochemical perfusate outlet end at the same time;
6) and 5) repeatedly circulating the pouring step for many times until the required curing strength is achieved.
3. The testing method of the temperature-controlled high-pressure biological solidification testing device as claimed in claim 2, wherein the solidification liquid in step 5) is composed of a bacterial liquid, a calcium chloride solution and a gelling liquid, wherein the gelling liquid is 0.5mol/L calcium acetate and 30g urea is added to each liter of the solution to dissolve the calcium acetate and the urea to obtain a mixed solution, the bacterial liquid is bacillus pasteurii, and the OD600 value is 2.268; the concentration of the calcium chloride solution is 0.05mol/L, and the ratio of the calcium chloride solution, the bacterial liquid and the gel liquid is 1: 5: 10.
4. The method for testing the bio-solidification testing apparatus under temperature-controlled high pressure as claimed in claim 2, wherein in the step 3), the pressure of the pressure chamber is controlled to be 1.0 to 15.0 MPa.
5. The method for testing the bio-solidification testing apparatus under temperature-controlled high pressure as claimed in claim 2, wherein the temperature during the testing in step 4) is 45-70 ℃.
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| CN114508321A (en) * | 2021-12-31 | 2022-05-17 | 中国石油天然气集团有限公司 | Method for reinforcing sea natural gas hydrate stratum by microorganism mineralization technology and application |
| CN114894566A (en) * | 2022-04-07 | 2022-08-12 | 中国矿业大学 | Preparation device and test method of microorganism curing sample under seepage-freeze thawing circulation effect |
| CN115629182A (en) * | 2022-10-13 | 2023-01-20 | 水利部交通运输部国家能源局南京水利科学研究院 | Microbial grouting reinforcement device considering temperature and confining pressure and use method |
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