CN110684541B - Application of graphene oxide in improving soil consolidation strength, composition and application method of graphene oxide - Google Patents
Application of graphene oxide in improving soil consolidation strength, composition and application method of graphene oxide Download PDFInfo
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Abstract
The invention provides application of graphene oxide in improving soil consolidation strength, a composition and a using method thereof, and relates to the technical field of microbial-induced calcium carbonate soil improvement. The graphene oxide can enable microorganisms to induce the rapid growth of calcium carbonate crystals in calcium carbonate, so that the yield of the calcium carbonate is increased; the size of calcium carbonate crystals can be changed, so that the consolidation of soil is facilitated, and the compressive strength of the soil is improved.
Description
Technical Field
The invention relates to the technical field of microbial-induced calcium carbonate soil improvement, in particular to application of graphene oxide in improving soil consolidation strength, a composition and a using method thereof.
Background
The microorganism-induced calcium carbonate consolidated soil is a main development trend in the field of soil improvement, and has the advantages that the action mechanism of the microorganism-induced calcium carbonate precipitation consolidated soil is as follows: urease decomposed by microorganisms can hydrolyze urea in a solution to generate carbonate ions, the carbonate ions react with calcium ions in the solution to generate calcium carbonate, and the calcium carbonate consolidates soil together by taking bacteria as a core point, so that the strength of the soil is improved, the material is harmless to the environment, is a novel green and environment-friendly material, and is a main development trend in the field of soil improvement.
However, in the use of the existing microorganism-induced calcium carbonate precipitation consolidation soil, the calcium ions cannot be completely consumed due to the insufficient hydrolysis of urea, so that the waste of resources is caused. The production of calcium carbonate is reduced due to insufficient reaction of calcium ions. Since the compressive strength of soil is in direct proportion to the yield of calcium carbonate, the soil cannot achieve the desired strength.
Disclosure of Invention
In view of the above, the present invention aims to provide an application of graphene oxide in improving soil consolidation strength, a composition for improving soil consolidation strength, and a use method thereof, wherein the composition of the present invention can improve total yield of calcium carbonate during microorganism-induced calcium carbonate induction, and improve compressive strength of soil.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides application of graphene oxide in improving soil consolidation strength.
The invention also provides a composition for improving the soil consolidation strength, which comprises the following raw materials:
the urease-producing microorganism solution comprises urease-producing microorganism solution, graphene oxide solution and cementing solution, wherein the effective viable count of urease-producing microorganisms in the urease-producing microorganism solution is 1 × 107～9×107cfu/m L, the concentration of the graphene oxide solution is 5-20 mg/L, the concentration of the cementing solution is 0.3-0.5 mol/L, and the volume ratio of the urease-producing microorganism solution to the graphene oxide solution to the cementing solution is (55-65) to (2-8) (220-260).
Preferably, the urease-producing microorganism comprises bacillus pasteurianus.
Preferably, the cementing liquid is obtained by mixing urea solution and calcium salt solution.
Preferably, the molar concentrations of the urea solution and the calcium salt solution are independently 0.3-0.5 mol/L.
Preferably, the volume ratio of the urea solution to the calcium salt solution is (100-140): 100-140.
Preferably, the calcium salt in the calcium salt solution comprises one or more of calcium chloride, calcium acetate, calcium nitrate and calcium lactate.
The invention also provides a using method of the composition in the technical scheme, which comprises the following steps: and mixing the urease-producing microorganism solution, the graphene oxide solution, the cementing solution and the sand, and then carrying out a soil consolidation reaction to improve the soil consolidation strength.
Preferably, the volume ratio of the mass of the sand to the urease-producing microorganism solution is (250-350) mg (50-70) m L.
Preferably, the ratio of the mass of the sand to the volume of the urease producing microbial solution is 300mg:60m L.
The invention provides an application of graphene oxide in improving soil consolidation strength, a composition for improving soil consolidation strength and a using method thereof. Graphene oxide is added into the microorganism-induced calcium carbonate, carboxyl in the graphene oxide can adsorb calcium ions, so that the graphene oxide is wrapped by the calcium ions, and then positively charged calcium ions adsorb urease-producing microorganisms, so that the urease-producing microorganisms can be fixed; the added graphene oxide improves the reaction rate of calcium ions and increases the yield of calcium carbonate; the added graphene oxide can change the size of calcium carbonate crystals on the premise of not changing the form of calcium carbonate, and is beneficial to the consolidation of soil, so that the compressive strength of the soil is improved.
Drawings
FIG. 1 is CaCO3Scanning electron microscope image and energy spectrum of crystal growth process, wherein (a) is CaCO in the presence of graphene oxide3Scanning electron microscope images of the crystal growth process; (b) is an energy spectrum diagram of the influence of the graphene oxide on the growth of the calcium carbonate crystal; wherein (B) the C, O and Ca atomic ratio of (a) the labeling regions A and B are recorded;
FIG. 2 is graphene oxide vs. Ca2+Concentration and CaCO3The total mass of the precipitate affects the result chart, wherein (A) is Ca under different graphene oxide concentrations2+Concentration; (B) at different bacterial concentrations (OD)600) Ca in the presence and absence of graphene oxide (10mg/L)2+Concentration; (C) as CaCO at different graphene oxide concentrations3The total mass of the precipitate; (D) at different bacterial concentrations (OD)600) CaCO in the presence and absence of graphene oxide (10mg/L)3Precipitating the total mass;
FIG. 3 is CaCO3A crystal XRD diffraction pattern, wherein (a) is CaCO without adding graphene oxide3Crystal XRD diffraction Pattern (OD)6000.25 part (b) is CaCO added with graphene oxide (10mg/L)3Crystal XRD diffraction Pattern (OD)600＝0.25)；
FIG. 4 shows the absence of graphene oxide under different bacterial concentrations, D600＝0.25(a)，D600＝0.50(b)，D600＝0.75(c)，D6001.0(D) and graphene oxide D600＝0.25(a1)，D 600＝0.50(b1)，D600＝0.75(c1)，D6001.0(d1) CaCO3Scanning electron microscope images of the crystals;
FIG. 5 shows bacteria (OD)6001.0) at 5 mg/L (a), 10mg/L (b),CaCO catalyzed at graphene oxide concentrations of 15 mg/L (c) and 20 mg/L (d)3Scanning electron microscope images of the crystals;
FIG. 6 is a graph of consolidated sand samples at different graphene oxide concentrations;
FIG. 7 is a graph of unconfined compressive strength results for consolidated sand at different graphene oxide concentrations.
Detailed Description
The invention provides application of graphene oxide in improving soil consolidation strength. The source of the graphene oxide is not particularly limited, and the graphene oxide can be obtained by adopting a conventional commercial product. In the invention, graphene oxide is added into microorganism-induced calcium carbonate, carboxyl in the graphene oxide can adsorb calcium ions, so that the graphene oxide is wrapped by the calcium ions, and then positively charged calcium ions adsorb urease-producing microorganisms, so that the urease-producing microorganisms can be fixed; the added graphene oxide improves the reaction rate of calcium ions and increases the yield of calcium carbonate; the added graphene oxide can change the size of calcium carbonate crystals on the premise of not changing the form of calcium carbonate, and is beneficial to the consolidation of soil, so that the compressive strength of the soil is improved. The soil of the present invention is not particularly limited in kind, and sandy gravel layer soil is preferable.
The invention provides a composition for improving soil consolidation strength, which comprises the following raw materials:
the urease-producing microorganism solution comprises urease-producing microorganism solution, graphene oxide solution and cementing solution, wherein the effective viable count of urease-producing microorganisms in the urease-producing microorganism solution is 1 × 107～9×107cfu/m L, the concentration of the graphene oxide solution is 5-20 mg/L, the concentration of the cementing solution is 0.3-0.5 mol/L, and the volume ratio of the urease-producing microorganism solution to the graphene oxide solution to the cementing solution is (55-65) to (2-8) (220-260).
The invention is not particularly limited to the kind of the urease producing microorganism, preferably Bacillus pasteurianus, more preferably Bacillus pasteurianus ATCC11859, and the Bacillus pasteurianus ATCC11859 may be a conventional commercially available product, in the invention, the effective viable count of the urease producing microorganism in the urease producing microorganism solution is 1 ×107～9×107cfu/ml, preferably 3.34 × 107～5.804×107cfu/ml. In the invention, urease decomposed by urease-producing microorganisms can hydrolyze urea in the cementing liquid to generate carbonate ions, the carbonate ions react with calcium ions in the cementing liquid to generate calcium carbonate, and the calcium carbonate uses bacteria as a core point to consolidate soil.
In the invention, the concentration of the graphene oxide solution is 5-20 mg/L, preferably 10-15 mg/L. in the invention, carboxyl in the graphene oxide can adsorb calcium ions, so that the graphene oxide is wrapped by the calcium ions, and then the positively charged calcium ions adsorb urease-producing microorganisms, so that the urease-producing microorganisms are fixed, the reaction rate of the calcium ions is improved, the yield of calcium carbonate is increased, the calcium carbonate crystals grow rapidly and have larger size, and the compressive strength of soil is obviously improved.
In the invention, the cementing liquid is preferably obtained by mixing a urea solution and a calcium salt solution, and the type of the calcium salt preferably comprises one or more of calcium chloride, calcium acetate, calcium nitrate and calcium lactate. In the invention, the cementing liquid provides carbonate and calcium ions for the urease-producing microorganisms to induce the calcium carbonate to consolidate the soil.
In the invention, the molar concentrations of the urea solution and the calcium salt solution are independently preferably 0.3-0.5 mol/L, the volume ratio of the urea solution to the calcium salt solution is preferably (100-140) to (100-140), the sources of the urea and the calcium salt are not particularly limited, and the urea and the calcium salt can be prepared from conventional commercial products.
The invention also provides a using method of the composition in the technical scheme, which comprises the following steps: and mixing the urease-producing microorganism solution, the graphene oxide solution and the cementing solution with sand, and then carrying out a soil consolidation reaction to improve the soil consolidation strength.
In the invention, the volume ratio of the sand mass to the urease-producing microorganism solution is preferably (250-350) mg, (50-70) m L, and more preferably 300mg:60m L.
In the present invention, the soil consolidated mould is preferably a full contact flexible mould, the diameter of the mould is preferably 50mm, and the height is preferably 100 mm. In the present invention, it is preferable to perform the soil consolidation reaction using a gas diffusion system. In the present invention, the full contact flexible mold is preferably made of geotextile through unconfined compression test samples.
The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Preparation of a suspension of bacillus pasteurii (ATCC 11859): aerobically culturing Bacillus pasteurii (ATCC11859) in 30 deg.C culture medium at 120 rpm for 48 hr, and centrifuging the culture at 4 deg.C 5434g for 8 min to obtain bacterial pellet; the bacterial pellet was diluted with deionized water to prepare bacterial suspensions (OD) of various concentrations6000.25, 0.5, 0.75 and 1.0).
Wherein the medium is prepared by mixing casein peptone (15 g/L), soy peptone (5 g/L), sodium chloride (5 g/L) and urea (20 g/L) into 1000m L deionized water, the final pH of the medium is about 7.3, and the medium is sterilized at 121 ℃ for 30 minutes.
The bacterial suspensions at different concentrations were 0.25(1.299 × 10) when the bacteria were diluted to 600nm7cfu/ml)、0.5(3.34×107cfu/ml)、0.75(5.804×107cfu/ml) and 1.0(8.59 × 10)7cfu/ml).
Example 2
Calcium carbonate precipitation 0.3 mol/L cementitious solutions were prepared by mixing 0.6 mol/L aqueous calcium chloride and 0.6 mol/L urea solutions different concentrations (OD) as prepared in example 16000.25, 0.5, 0.75 and 1.0) calcium carbonate precipitation was carried out at 25 ℃ in beakers containing 60 ml of the bacterial suspension and 240 ml of a binding solution consisting of 120m L calcium chloride and 120m L urea solution, respectively, at a concentration of 0.3 mol/L of the binding solutionAt different bacterial concentrations (OD)6000.25, 0.5, 0.75 and 1.0), precipitation was performed without addition of graphene oxide and with addition of 2 ml of 10mg/L graphene oxide, when the bacterial concentration was equal to OD600At 1.0, the same calcium carbonate precipitation was performed at different concentrations of graphene oxide (5, 10, 15 and 20 mg/L) and cement (0.3 mol/L).
Soil consolidation: the bacterial suspension prepared in the embodiment 1, the graphene oxide and the cementing liquid in the embodiment 2 and 300g of sand are mixed and then subjected to a consolidation reaction, so that the soil consolidation strength is improved.
The data of the results of the addition of graphene oxide on the microbial-induced precipitation of calcium carbonate are as follows:
the calcium carbonate precipitated calcium carbonate crystal growth mechanism and the influence of graphene oxide result: in the process of calcium carbonate crystal growth in the presence of graphene oxide, when urea and calcium chloride are used, calcium carbonate crystals start to grow on the surface of graphene oxide (fig. 1 (a)). The effect of graphene oxide on calcium carbonate crystal growth was further characterized by EDS, which showed C, O and Ca atomic ratios of 68:32 and 53:45:2 for regions a and B (fig. 1(a)), respectively (fig. 1 (B)). The result shows that the graphene oxide can adsorb Ca in the process of microorganism-induced calcium carbonate2+Ion, Ca2+The ions can adsorb bacteria, CaCO3Crystal growth is affected by graphene oxide. Indicating that the bacteria can be immobilized.
Graphene oxide on Ca2+Concentration and CaCO3Total mass of precipitate influence results plot: ca at different graphene oxide concentrations2+The change in concentration of Ca in the presence of graphene oxide is shown in FIG. 2(A)2+Decreases more rapidly than in the absence of graphene oxide, Ca is present at graphene oxide concentrations of 10, 15 and 20 mg/L2+The change in concentration is substantially the same. The effect of graphene oxide becomes more pronounced at different bacterial concentrations (fig. 2 (B)). Ca increases with the concentration of bacteria2+The reaction rate of (3) increases. When the concentration of bacteria is OD6000.25 hour, first 24 hours Ca2+The change in concentration was essentially the same as in the absence of graphene oxide, but after 24 hours Ca was present in the presence of graphene oxide2+The concentration decreased faster than without the graphene oxide. Initially, when the bacterial concentration is OD6000.5, 0.75 and 1.0, the presence of graphene oxide makes Ca2+The concentration drops more rapidly. The above results indicate that graphene oxide favors Ca2+And (4) reacting. Although in the absence of graphene oxide, Ca2+Not completely deposited, but in the case of graphene oxide, Ca was present after 36 hours2+And (4) completely depositing. FIG. 2(C) shows CaCO in the presence of graphene oxide3Total mass of precipitate increased by at least 53%. FIG. 2(D) shows the total mass of bacterial urease catalyzing the precipitation of calcium carbonate at various bacterial concentrations with graphene oxide (10mg/L) and without graphene oxide CaCO3Precipitation increases with increasing bacterial concentration. When the concentration of bacteria is OD6000.25, 0.5, 0.75 and 1.0 CaCO in the presence of graphene oxide (10mg/L) compared to no graphene oxide3Precipitation was increased by at least 171%, 73%, 33% and 26%, respectively. At a bacterial concentration of 0.5, Ca is present2+Complete deposition of CaCO3The total mass of the precipitate reaches a maximum.
CaCO3Crystal XRD diffraction pattern: the polymorphism of calcium carbonate crystals catalyzed by bacterial urease was analyzed by XRD (fig. 3). When the bacterial concentration is 0.25, calcite is present regardless of the addition of graphene oxide. Without the addition of Go, a small amount of vaterite was obtained. More stable crystals are obtained in the presence of graphene oxide.
The CaCO prepared at different bacterial concentrations was observed by scanning electron microscopy (FIG. 4(a, b, c, and d))3Morphology of the crystal. As shown in FIGS. 4a, b, c and d, CaCO3The size of the crystal is respectively in the range of 7-22 microns, 18-48 microns, 17-38 microns and 24-113 microns. At lower bacterial concentrations, regular diamond crystals were obtained. When the concentration of bacteria is OD600At 0.25, vaterite was produced (fig. 4 (a)). When the concentration of bacteria is OD600At 1.0, the calcium carbonate crystals agglomerated. An important feature of this phenomenon is that as the concentration of bacteria increases, the size of the crystals increases, since there is sufficient reaction massCa2+。
Scanning electron microscopy (FIG. 4(a1, b1, c1, and d1)) was used to observe CaCO prepared at different bacterial concentrations of graphene oxide 10mg/L3Morphology of the crystal. As shown in FIGS. 4a1, b1, c1 and d1, CaCO3The size of the crystal is respectively in the range of 24-53 microns, 17-67 microns, 38-72 microns and 28-113 microns. CaCO in the presence of different bacterial concentrations and graphene oxide (10mg/l)3The crystals are larger than those obtained in the absence. This is because the bacteria adsorb Ca on the edge of graphene oxide2+Another important phenomenon is that in the presence of 10mg/L graphene oxide, the size of the crystal decreases with increasing bacterial concentration, since graphene oxide can act as a nucleation site due to the presence of sufficient Ca2+，CaCO3The crystals can be grown continuously, thereby producing larger CaCO3And (4) crystals. However, at higher nucleation concentrations, there is not enough Ca2+Thus, without single crystal growth, large amounts of small CaCO are produced3And (4) crystals. The results show that the use of graphene oxide in the process of microbial induction of calcium carbonate precipitation results in larger size of calcium carbonate crystals, so that the unconfined compressive strength of the consolidated soil is significantly improved.
CaCO at different graphene oxide concentrations3The morphology of the crystals is shown in fig. 5. as the concentration of graphene oxide increases, the size of the calcium carbonate crystals decreases.
Samples of consolidated sand after 6 days of reaction of the bacterial suspension, the cementing fluid and the sand at different graphene oxide concentrations are shown in fig. 6, better integrity and compaction was observed with graphene oxide than without graphene oxide, an unconfined compressive strength test is shown in fig. 7, where it is important that the unconfined compressive strength of the consolidated sand increases by 100% at maximum in the presence of 15 mg/L graphene oxide, the unconfined compressive strength of the consolidated sand decreases when the graphene oxide concentration is 20 mg/L, due to the presence of spherical crystals (fig. 6 (d)).
From the results of the above embodiments, it can be seen that the graphene oxide is added to the microorganism-induced calcium carbonate, so that the graphene oxide can adsorb calcium ions, and the graphene oxide is wrapped by the calcium ions, and then the positively charged calcium ions adsorb the bacillus pasteurii, so that the bacillus pasteurii can be immobilized; the reaction rate of calcium ions can be improved, and the yield of calcium carbonate is increased; on the premise of not changing the form of calcium carbonate, the calcium carbonate crystals become large, which is beneficial to the consolidation of soil, thereby improving the compressive strength of the soil.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. Use of graphene oxide for increasing the consolidation strength of soil, wherein the graphene oxide is provided in the form of a composition; the composition comprises the following raw materials: producing urease microorganism solution, graphene oxide solution and cementing solution;
the effective viable count of the urease-producing microorganisms in the urease-producing microorganism solution is 1 × 107～9×107cfu/mL；
The concentration of the graphene oxide solution is 5-20 mg/L;
the concentration of the cementing liquid is 0.3-0.5 mol/L;
the volume ratio of the urease-producing microorganism solution to the graphene oxide solution to the cementing solution is (55-65): (2-8) (220-260).
2. A composition for improving soil consolidation strength, which is characterized by comprising the following raw materials: producing urease microorganism solution, graphene oxide solution and cementing solution; the urease-producing microorganisms in the urease-producing microorganism solutionThe effective viable count is 1 × 107～9×107cfu/m L, wherein the concentration of the graphene oxide solution is 5-20 mg/L;
the concentration of the cementing liquid is 0.3-0.5 mol/L, and the volume ratio of the urease-producing microorganism solution to the graphene oxide solution to the cementing liquid is (55-65): (2-8) (220-260).
3. The composition of claim 2, wherein the urease-producing microorganism comprises bacillus pasteurii.
4. The composition according to claim 2, wherein the cementing liquid is obtained by mixing a urea solution and a calcium salt solution.
5. The composition as claimed in claim 4, wherein the molar concentrations of the urea solution and the calcium salt solution are 0.3-0.5 mol/L, respectively.
6. The composition as claimed in claim 4 or 5, wherein the volume ratio of the urea solution to the calcium salt solution is (100-140): 100-140.
7. The composition of claim 4, wherein the calcium salt in the calcium salt solution comprises one or more of calcium chloride, calcium acetate, calcium nitrate, and calcium lactate.
8. A method of using the composition of claim 2, comprising: and mixing the urease-producing microorganism solution, the graphene oxide solution, the cementing solution and the sand, and then carrying out a soil consolidation reaction to improve the soil consolidation strength.
9. The use method of claim 8, wherein the ratio of the mass of the sand to the volume of the urease-producing microbial solution is (250-350) mg (50-70) m L.
10. The use of the method according to claim 9, wherein the ratio of the mass of the sand to the volume of the urease producing microbial solution is 300mg:60m L.
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