Molybdenum-based nanocomposite and preparation method and application thereof

Abstract

The invention provides a molybdenum-based nano composite material as well as a preparation method and application thereof. The molybdenum-based nano composite material comprises molybdenum disulfide nanoflowers, molybdenum disulfide nanosheets, molybdenum disulfide nanodots, molybdenum oxide nanoparticles, carbon-based molybdenum single atoms and molybdenum-based polyoxometallate nanoparticles. The molybdenum-based nano composite material mediated and adjustable by the physiological microenvironment is designed, the material integrates the efficient antibacterial performance similar to that of traditional antibiotics, intestinal flora disorder caused by use of the antibiotics can be remarkably recovered, the relative abundance of probiotics is improved, the problem of intestinal flora imbalance caused by abuse of the antibiotics is solved, and the effect of improving the intestinal flora imbalance is achieved. The application effect of far-end tumor treatment can be achieved. The material is suitable for industrialization and has a huge market demand prospect.

Description

Technical Field

[0001] The present invention belongs to the field of chemistry and drug-carrying technology, and specifically relates to a molybdenum-based nanocomposite material and a preparation method and application thereof. Background Art

[0002] Bacterial infections often trigger a variety of diseases, and antibiotics can effectively control and treat diseases caused by bacterial infections. However, improper and excessive use of antibiotics not only leads to the development of bacterial resistance but also contributes to the occurrence and progression of various diseases. Clinical studies have shown that the misuse of antibiotics can exacerbate the occurrence and progression of tumors, and the type and duration of antibiotic use are positively correlated with tumor progression. While studying these causes, scientists have discovered that intestinal flora disturbances caused by antibiotic misuse may be a significant contributor to disease progression.

[0003] CN116836882A relates to a microbial agent of Bacteroides monomorpha, which can promote the recovery of α diversity, Bifidobacterium, Enterobacterium, etc. in the intestinal microbiome of mice after short-term broad-spectrum antibiotic perturbation, so as to achieve the effects of prevention and treatment; however, in actual application, the preservation problem of the microbial agent and its degradation by the gastric fluid environment often reduce the drug effect, making it difficult to achieve on-demand drug release. Nanoparticles have excellent safety and good biocompatibility, and are easy to penetrate into cells, effectively overcoming the defects of some small molecule preparations such as poor bioselectivity, low utilization rate, and serious adverse reactions. Molybdenum-based nanomaterials, such as molybdenum disulfide (MoS2), are a typical graphene-like two-dimensional transition metal sulfide. Due to its advantages such as low cost, high stability, easy large-scale production, good biosafety, and adjustable catalytic activity, it has shown broad application prospects in the biomedical field. CN114177291A relates to a drug delivery system based on molybdenum disulfide nanoparticles. This system has the characteristics of tumor microenvironment response and good stability, which can achieve targeted tumor treatment. However, scientists have only focused on the excellent drug-loading capacity of molybdenum-based nanomaterials, ignoring whether they can affect tumor progression by regulating intestinal flora.

[0004] Therefore, there is an urgent need to design a molybdenum-based nanocomposite material to restore the intestinal flora disorder caused by the use of antibiotics in order to achieve the application effect of remote tumor treatment. Summary of the Invention

[0005] To address the shortcomings of the existing technology, the present invention aims to provide a molybdenum-based nanocomposite material, its preparation method, and its application. This invention designs a molybdenum-based nanocomposite material that is tunable by physiological microenvironmental regulation. This material combines highly effective antimicrobial properties similar to those of traditional antibiotics. It can significantly restore intestinal flora disturbances caused by antibiotic use, increase the relative abundance of probiotics, overcome the imbalance in intestinal flora caused by antibiotic overuse, and achieve therapeutic effects in distal tumors. This material is suitable for industrialization and has significant market demand.

[0006] In order to achieve the purpose of the invention, the present invention adopts the following technical solutions:

[0007] In a first aspect, the present invention provides a molybdenum-based nanocomposite material, which includes molybdenum disulfide nanoflowers, molybdenum disulfide nanosheets, molybdenum disulfide nanodots, molybdenum oxide nanoparticles, carbon-based molybdenum single atoms and molybdenum-based polyoxometalate nanoparticles.

[0008] This invention has designed a molybdenum-based nanocomposite material that is tunable through physiological microenvironmental regulation. This material combines highly effective antimicrobial properties similar to those of traditional antibiotics. It can significantly restore intestinal flora disturbances caused by antibiotic use, increase the relative abundance of probiotics, and overcome the imbalance in intestinal flora caused by antibiotic overuse, achieving therapeutic benefits for distal tumors. This material is suitable for industrialization and has significant market demand.

[0009] In the present invention, the combination of molybdenum disulfide nanoflowers, molybdenum disulfide nanosheets, molybdenum disulfide nanodots, molybdenum oxide nanoparticles, carbon-based molybdenum single atoms and molybdenum-based polyoxometalate nanoparticles helps to improve the intestinal flora disorder caused by the use of antibiotics through molybdenum-based nanomaterials with different particle sizes or structures.

[0010] As a preferred technical solution of the present invention, the non-molybdenum metal element in the molybdenum-based polyoxometalate nanoparticles includes any one of manganese, cobalt or bismuth, or a combination of at least two of them.

[0011] As a preferred technical solution of the present invention, the particle size D50 of the molybdenum-based nanocomposite material is 10-100 nm, for example, 10 nm, 20 nm, 30 nm, 40 nm, 50 nm, 60 nm, 70 nm, 80 nm, 90 nm or 100 nm, etc. However, the particle size D50 is not limited to the values listed above, and other values not listed within the numerical range are also applicable.

[0012] In the present invention, if the particle size D50 of the molybdenum-based nanocomposite material is too small, it is not conducive to the molybdenum-based nanocomposite material playing a role in the intestine; if the particle size D50 of the molybdenum-based nanocomposite material is too large, the molybdenum-based nanocomposite material will seriously agglomerate, which is not conducive to its function.

[0013] In a second aspect, the present invention provides a method for preparing the molybdenum-based nanocomposite material as described in the first aspect, the preparation method comprising the following steps:

[0014] (1) mixing a molybdenum source and an organic solvent to obtain a dispersion;

[0015] (2) subjecting the dispersion to a microwave hydrothermal reaction to obtain the molybdenum-based nanocomposite material.

[0016] In the present invention, microwave hydrothermal reaction can synthesize typical molybdenum-based nanoflower morphology, while oven hydrothermal method will cause serious agglomeration of molybdenum-based nanomaterials and fail to form a specific morphology. Commercialized molybdenum disulfide presents a blocky morphology at the micron level.

[0017] As a preferred technical solution of the present invention, the molybdenum source in step (1) is ammonium tetrathiomolybdate.

[0018] Preferably, the organic solvent in step (1) is N,N-dimethylformamide.

[0019] Preferably, the solid-to-liquid ratio of the molybdenum source and the organic solvent in step (1) is (0.006-0.012) g:(20-50) mL, wherein the selection range of the molybdenum source "(0.006-0.012) g" can be, for example, 0.006 g, 0.008 g, 0.01 g or 0.012 g, and the selection range of the organic solvent "(20-50) mL" can be, for example, 20 mL, 25 mL, 30 mL, 35 mL, 40 mL, 45 mL or 50 mL. However, the present invention is not limited to the listed values, and other values not listed within the numerical range are also applicable.

[0020] In the present invention, if the mass of the molybdenum source is too large, the morphology of the molybdenum-based nanomaterial will be changed.

[0021] As a preferred technical solution of the present invention, the temperature of the microwave hydrothermal reaction in step (2) is 150-200°C, for example, it can be 150°C, 160°C, 170°C, 180°C, 190°C or 200°C.

[0022] Preferably, the microwave hydrothermal reaction time in step (2) is 12-20 h, for example, 12 h, 14 h, 16 h, 18 h or 20 h, etc. However, this is not limited to the listed values, and other values not listed within this numerical range are also applicable.

[0023] In the present invention, if the microwave hydrothermal reaction time is too short, the dispersibility of the molybdenum-based nanomaterial will be affected. After the reaction time is 12-20 hours, a molybdenum-based nanoflower morphology with good dispersibility can be obtained.

[0024] As a preferred technical solution of the present invention, the preparation method comprises the following steps:

[0025] (1) dissolving ammonium tetrathiomolybdate in N,N-dimethylformamide and ultrasonicating for 30-60 min (e.g., 30 min, 40 min, 50 min, or 60 min) to obtain a dispersion;

[0026] Wherein, the solid-liquid ratio of ammonium tetrathiomolybdate and N,N-dimethylformamide is (0.006-0.012) g: (20-50) mL;

[0027] (2) transferring the dispersion into a microwave reactor, performing a microwave hydrothermal reaction at 150-200° C. for 12-20 h, cooling the dispersion to room temperature after the reaction, and then washing and centrifuging the dispersion to obtain a precipitate. The precipitate is then dried at 40-80° C. (for example, 40° C., 50° C., 60° C., 70° C., or 80° C.) for 4-8 h (for example, 4 h, 5 h, 6 h, 7 h, or 8 h, etc.) to obtain the molybdenum-based nanocomposite material.

[0028] In a third aspect, the present invention provides an application of the molybdenum-based nanocomposite material as described in the first aspect, wherein the molybdenum-based nanocomposite material is used to improve intestinal flora disorders caused by the use of antibiotics.

[0029] As a preferred technical solution of the present invention, the application objects of the molybdenum-based nanocomposite material include any one of rodents, rabbits, dogs, pigs, sheep or monkeys.

[0030] The present invention does not limit the type of the rodent. For example, the rodent may be a mouse, a rat, a hamster or a guinea pig.

[0031] Preferably, the molybdenum-based nanocomposite material is applied by gavage or feeding.

[0032] The numerical range described in the present invention includes not only the point values listed above, but also any point values between the above numerical ranges that are not listed. Due to space limitations and for the sake of simplicity, the present invention no longer exhaustively lists the specific point values included in the range.

[0033] Compared with the prior art, the present invention has the following beneficial effects:

[0034] (1) The present invention designs a molybdenum-based nanocomposite material that is regulated by the physiological microenvironment. This material combines high-efficiency antibacterial properties similar to those of traditional antibiotics, can significantly restore intestinal flora disorders caused by the use of antibiotics, increase the relative abundance of probiotics, overcome the problem of intestinal flora imbalance caused by the abuse of antibiotics, and achieve the application effect of remote tumor treatment;

[0035] (2) The preparation method provided by the present invention is easy to control, low in cost, easy to promote and apply, and is conducive to the development of personalized medicine. It is also very suitable for industrialization, satisfies the general public, has huge market demand prospects, and can bring huge economic and social benefits. BRIEF DESCRIPTION OF THE DRAWINGS

[0036] Figure 1 This is the SEM image of molybdenum disulfide nanoflowers in the molybdenum-based nanocomposite material prepared in Example 1.

[0037] Figure 2 This is a TEM image of molybdenum disulfide nanoflowers in the molybdenum-based nanocomposite material prepared in Example 1.

[0038] Figure 3 This is a TEM image of carbon-based molybdenum single atoms in the molybdenum-based nanocomposite material prepared in Example 1.

[0039] Figure 4 This is a spherical aberration-corrected transmission electron microscopy image of a carbon-based molybdenum single atom in the molybdenum-based nanocomposite material prepared in Example 1.

[0040] Figure 5 This is the SEM image of the molybdenum-based nanocomposite material prepared in Example 5-6.

[0041] Figure 6 These are SEM images of the molybdenum-based nanocomposites prepared in Examples 7-11.

[0042] Figure 7 The SEM images of the molybdenum-based nanomaterials provided for Comparative Examples 1-2.

[0043] Figure 8 This is an analysis chart of the changes in intestinal flora diversity of each group of mice in the application method provided in Application Example 1.

[0044] Figure 9 This is an analysis chart of the changes in the relative abundance of intestinal strains in each group of mice in the application method provided in Application Example 1.

[0045] Figure 10 This is an analysis diagram of the main components of the intestinal flora of each group of mice in the application method provided in Application Example 2.

[0046] Figure 11 This is an analysis chart of the changes in intestinal flora diversity of each group of mice in the application method provided in Application Example 2.

[0047] Figure 12 This is an analysis chart of the changes in the relative abundance of intestinal strains in each group of mice in the application method provided in Application Example 2. DETAILED DESCRIPTION

[0048] The technical solution of the present invention is further described below by way of specific embodiments. It should be understood by those skilled in the art that the embodiments are merely to help understand the present invention and should not be regarded as specific limitations of the present invention.

[0049] It should be noted that the room temperature below refers to 25°C.

[0050] Example 1

[0051] This embodiment provides a molybdenum-based nanocomposite material, comprising molybdenum disulfide nanoflowers, molybdenum disulfide nanosheets, molybdenum disulfide nanodots, molybdenum oxide nanoparticles, carbon-based molybdenum single atoms, and molybdenum-based polyoxometalate nanoparticles;

[0052] The molybdenum-based polyoxometalate nanoparticles are molybdenum manganese oxometalate;

[0053] The particle size D50 of the molybdenum-based nanocomposite material is 50 nm.

[0054] This embodiment also provides a method for preparing the above-mentioned molybdenum-based nanocomposite material, which comprises the following steps:

[0055] (1) Dissolve 0.012 g of ammonium tetrathiomolybdate in 30 mL of N,N-dimethylformamide and ultrasonicate for 40 min to obtain a dispersion;

[0056] Among them, the solid-liquid ratio of ammonium tetrathiomolybdate and N,N-dimethylformamide is 0.012g:30mL;

[0057] (2) The dispersion was transferred to a 35 mL microwave reactor and subjected to microwave hydrothermal reaction at 180° C. under stirring for 12 h. After the reaction was completed, the dispersion was cooled to room temperature and then washed with deionized water for 3 times. The precipitate obtained by centrifugation was dried in an oven at 60° C. for 6 h to obtain the molybdenum-based nanocomposite material.

[0058] Figure 1 The SEM image of the molybdenum disulfide nanoflowers in the molybdenum-based nanocomposite material prepared in this embodiment is shown. As can be seen from the image, the molybdenum disulfide nanoflowers present a dispersed nanoflower structure.

[0059] Figure 2 The TEM image of the molybdenum disulfide nanoflowers in the molybdenum-based nanocomposite material prepared in this embodiment is shown. As can be seen from the figure, the molybdenum disulfide nanoflowers present a three-dimensional nanoflower structure, proving the successful preparation of the material.

[0060] Figure 3 and Figure 4The TEM image and spherical aberration-corrected transmission electron microscope image of the carbon-based molybdenum single atom in the molybdenum-based nanocomposite prepared in this embodiment are respectively shown. It can be seen from the figures that the carbon-based molybdenum single atom is successfully prepared.

[0061] Example 2

[0062] This embodiment provides a molybdenum-based nanocomposite material, comprising molybdenum disulfide nanoflowers, molybdenum disulfide nanosheets, molybdenum disulfide nanodots, molybdenum oxide nanoparticles, carbon-based molybdenum single atoms, and molybdenum-based polyoxometalate nanoparticles;

[0063] The molybdenum-based polyoxometalate nanoparticles are molybdenum bismuth oxometalate;

[0064] The particle size D50 of the molybdenum-based nanocomposite material is 40 nm.

[0065] This embodiment also provides a method for preparing the above-mentioned molybdenum-based nanocomposite material, which comprises the following steps:

[0066] (1) Dissolve 0.012 g of ammonium tetrathiomolybdate in 30 mL of N,N-dimethylformamide and ultrasonicate for 40 min to obtain a dispersion;

[0067] Among them, the solid-liquid ratio of ammonium tetrathiomolybdate and N,N-dimethylformamide is 0.012g:30mL;

[0068] (2) The dispersion was transferred to a 35 mL microwave reactor and subjected to microwave hydrothermal reaction at 190° C. under stirring for 14 h. After the reaction was completed, the dispersion was cooled to room temperature and then washed with deionized water for 3 times. The precipitate obtained by centrifugation was dried in an oven at 60° C. for 6 h to obtain the molybdenum-based nanocomposite material.

[0069] Example 3

[0070] This embodiment provides a molybdenum-based nanocomposite material, comprising molybdenum disulfide nanoflowers, molybdenum disulfide nanosheets, molybdenum disulfide nanodots, molybdenum oxide nanoparticles, carbon-based molybdenum single atoms, and molybdenum-based polyoxometalate nanoparticles;

[0071] The molybdenum-based polyoxometalate nanoparticles are molybdenum manganese oxometalate;

[0072] The particle size D50 of the molybdenum-based nanocomposite material is 80 nm.

[0073] This embodiment also provides a method for preparing the above-mentioned molybdenum-based nanocomposite material, which comprises the following steps:

[0074] (1) Dissolve 0.006 g of ammonium tetrathiomolybdate in 40 mL of N,N-dimethylformamide and ultrasonicate for 40 min to obtain a dispersion;

[0075] Among them, the solid-liquid ratio of ammonium tetrathiomolybdate and N,N-dimethylformamide is 0.006g:40mL;

[0076] (2) The dispersion was transferred to a 35 mL microwave reactor and subjected to microwave hydrothermal reaction at 200° C. under stirring for 12 h. After the reaction was completed, the dispersion was cooled to room temperature and then washed with deionized water for 3 times. The precipitate obtained by centrifugation was dried in an oven at 60° C. for 6 h to obtain the molybdenum-based nanocomposite material.

[0077] Example 4

[0078] The difference between this embodiment and embodiment 1 is that the amount of ammonium tetrathiomolybdate added in step (1) is 0.004 g.

[0079] The rest of the preparation methods and parameters remained the same as in Example 1.

[0080] Example 5

[0081] The difference between this embodiment and embodiment 1 is that the amount of ammonium tetrathiomolybdate added in step (1) is 0.024 g.

[0082] The rest of the preparation methods and parameters remained the same as in Example 1.

[0083] Example 6

[0084] The difference between this embodiment and embodiment 1 is that the amount of ammonium tetrathiomolybdate added in step (1) is 0.048 g.

[0085] The rest of the preparation methods and parameters remained the same as in Example 1.

[0086] Figure 5 The SEM images of the molybdenum-based nanocomposites prepared in Example 5-6 are shown. Figure 5 and Figure 1 It can be seen from the comparison that if the amount of molybdenum-based nanocomposites added is too much, the molybdenum-based nanocomposites will become more agglomerated.

[0087] Example 7

[0088] The difference between this embodiment and embodiment 1 is that the reaction time in step (2) is 3 h.

[0089] The rest of the preparation methods and parameters remained the same as in Example 1.

[0090] Example 8

[0091] The difference between this embodiment and embodiment 1 is that the reaction time in step (2) is 6 h.

[0092] The rest of the preparation methods and parameters remained the same as in Example 1.

[0093] Example 9

[0094] The difference between this embodiment and embodiment 1 is that the reaction time in step (2) is 9 hours.

[0095] The rest of the preparation methods and parameters remained the same as in Example 1.

[0096] Example 10

[0097] The difference between this embodiment and embodiment 1 is that the reaction time in step (2) is 10 h.

[0098] The rest of the preparation methods and parameters remained the same as in Example 1.

[0099] Example 11

[0100] The difference between this embodiment and embodiment 1 is that the reaction time in step (2) is 11 h.

[0101] The rest of the preparation methods and parameters remained the same as in Example 1.

[0102] Figure 6 The SEM images of the molybdenum-based nanocomposites prepared in Examples 7-11 are shown. Figure 6 and Figure 1 The comparison shows that the molybdenum-based nanocomposite material synthesized after 3 h of reaction is mainly in a clustered state. As the reaction time increases, the material becomes more dispersed. After 12 h of reaction, a molybdenum disulfide nanoflower structure with better dispersion appears.

[0103] Example 12

[0104] The difference between this embodiment and embodiment 1 is that the particle size D50 of the molybdenum-based nanocomposite material is 5 nm.

[0105] The rest of the preparation methods and parameters remained the same as in Example 1.

[0106] Example 13

[0107] The difference between this embodiment and embodiment 1 is that the particle size D50 of the molybdenum-based nanocomposite material is 150 nm.

[0108] The rest of the preparation methods and parameters remained the same as in Example 1.

[0109] Comparative Example 1

[0110] The difference between this comparative example and Example 1 is that the microwave reactor in step (2) is replaced by an oven, and the hydrothermal reaction is carried out in the oven.

[0111] The rest of the preparation methods and parameters remained the same as in Example 1.

[0112] Comparative Example 2

[0113] This comparative example provides a commercial molybdenum-based nanomaterial.

[0114] Figure 7 Shown are SEM images of the molybdenum-based nanomaterials provided in Comparative Examples 1-2, as shown in FIG. Figure 1 From the comparison, it can be seen that the molybdenum-based nanocomposites synthesized by microwave hydrothermal method have dispersed molybdenum disulfide nanoflower structures, the molybdenum-based nanomaterials synthesized by oven hydrothermal method are severely agglomerated and have no specific morphology, and the commercial molybdenum-based nanomaterials mainly present blocky morphology at the micron level.

[0115] Application Example 1

[0116] This application example provides an application of a molybdenum-based nanocomposite material, wherein the molybdenum-based nanocomposite material is applied to an antibiotic-resistant mouse model, and the application method comprises the following steps:

[0117] (1) C57BL / 6N mice were gavaged with the multidrug-resistant strain Helicobacter pylori CCPM(A)-P-360159, once every other day for six consecutive times, and then kept in the environment to establish a Helicobacter pylori infection model in mice.

[0118] (2) 26 days after inoculation with Helicobacter pylori, the mice were divided into 4 groups: an uninfected group, an infected group (treated with phosphate buffer), a triple (omeprazole + amoxicillin + clarithromycin) treatment group, and a quadruple (omeprazole + amoxicillin + clarithromycin + the molybdenum-based nanocomposite material provided in Example 1) treatment group. The mice were given the drug by gavage once every other day. After 4 consecutive gavages, the intestinal feces of the mice were collected for microbial diversity sequencing (16s).

[0119] Figure 8 The figure shows the changes in the diversity of the intestinal flora of each group of mice in the application method provided in this application example. It can be seen from the figure that antibiotic treatment causes a decrease in the diversity of the intestinal flora of mice, and the addition of molybdenum-based nanomaterials can significantly restore the diversity of the intestinal flora of mice.

[0120] Figure 9The figure shows the change analysis of the relative abundance of intestinal strains in each group of mice in the application method provided in this application example. It can be seen from the figure that antibiotic treatment causes changes in the relative abundance of intestinal strains in mice. After the addition of molybdenum-based nanomaterials, the relative abundance of intestinal strains in mice can be significantly restored. Among them, the abundance of two types of intestinal probiotics, Dubosiella and Akkermansia muciniphila, is significantly increased, indicating that the present invention can significantly improve the intestinal flora disorder caused by antibiotics.

[0121] Application Example 2

[0122] This application example provides an application of a molybdenum-based nanocomposite material, wherein the molybdenum-based nanocomposite material is applied to an antibiotic-resistant mouse model, and the application method comprises the following steps:

[0123] (1) C57BL / 6N mice were randomly divided into four groups: a control group, an antibiotic (neomycin sulfate and clarithromycin) group, an antibiotic + platinum-based nanocomposite (provided in Example 1) group, and a platinum-based nanocomposite (provided in Example 1) group;

[0124] (2) Mice were treated with antibiotics and molybdenum-based nanocomposites by gavage, once every other day for 5 times in a row. The control group was treated with normal saline. The intestinal feces of the mice were then collected for microbial diversity sequencing (16s).

[0125] Figure 10 An analysis diagram of the main components of the intestinal flora of each group of mice in the application method provided in this application example is shown. It can be seen from the figure that compared with the antibiotic group, the flora composition of the molybdenum-based nanocomposite group and the antibiotic + molybdenum-based nanocomposite group is closer to that of the control group.

[0126] Figure 11 An analysis chart showing changes in intestinal flora diversity of each group of mice in the application method provided in this application example is shown. As can be seen from the figure, the flora diversity of the antibiotic group is significantly reduced, and the combined administration of molybdenum-based nanocomposites can significantly restore the diversity of intestinal flora, proving that the present invention can significantly improve the changes in intestinal flora diversity caused by antibiotics.

[0127] Figure 12 The figure shows the change analysis of the relative abundance of intestinal strains in each group of mice in the application method provided in this application example. It can be seen from the figure that antibiotic treatment causes changes in the relative abundance of intestinal strains in mice. After the addition of molybdenum-based nanocomposites, the relative abundance of intestinal strains in mice can be significantly restored. Among them, the abundance of intestinal probiotic Dubosiella is significantly increased, which proves that the present invention can significantly improve the intestinal flora disorder caused by antibiotics.

[0128] Application Example 3-14

[0129] The application methods provided in Application Examples 3-14 are different from those in Application Example 1 in that the molybdenum-based nanocomposites are provided by Examples 2-13, respectively.

[0130] Other application methods and parameters are consistent with those in Application Example 1.

[0131] Application Comparative Example 1-2

[0132] The difference between the application methods provided in Comparative Examples 1-2 and Application Example 1 is that the molybdenum-based nanocomposites are provided by Comparative Examples 1-2, respectively.

[0133] Other application methods and parameters are consistent with those in Application Example 1.

[0134] analyze:

[0135] It can be seen from Application Examples 1 and 6-7 that the more molybdenum-based nanocomposites are added, the more agglomerated the molybdenum-based nanocomposites will be, and the changes in the diversity of mouse intestinal flora and the relative abundance of mouse intestinal strains will be small, with no significant difference from the triple treatment group.

[0136] It can be seen from Application Examples 1 and 8-12 that the shorter the reaction time, the more agglomerated the molybdenum-based nanocomposite materials will be, and the changes in the diversity of mouse intestinal flora and the relative abundance of mouse intestinal strains will be smaller, with no significant difference from the triple treatment group.

[0137] It can be seen from Application Examples 1 and 13-14 that if the particle size D50 of the molybdenum-based nanocomposite material is too small or too large, it is not conducive to the effect of the molybdenum-based nanocomposite material in the intestine, but it has little effect on the diversity of mouse intestinal flora and the relative abundance of mouse intestinal strains.

[0138] It can be seen from Application Example 1 and Application Comparison Examples 1-2 that replacing the microwave reactor with an oven and conducting a hydrothermal reaction in the oven will cause the molybdenum-based nano-composite material to severely agglomerate and have no specific morphology, and the diversity of mouse intestinal flora and the relative abundance of mouse intestinal strains will change little; while the commercial molybdenum-based nanomaterials mainly present a block morphology at the micron level, which has little effect on the diversity of mouse intestinal flora and the relative abundance of mouse intestinal strains.

[0139] The applicant states that while the above-described embodiments illustrate the process of the present invention, the present invention is not limited to the above-described process steps, nor does it imply that the present invention must rely on the above-described process steps for implementation. Those skilled in the art will appreciate that any improvements to the present invention, equivalent substitutions for the raw materials used, additions of auxiliary components, and selection of specific methods, etc., fall within the scope of protection and disclosure of the present invention.

Claims

1. A molybdenum-based nanocomposite material, characterized in that: The molybdenum-based nanocomposite material comprises molybdenum disulfide nanoflowers, molybdenum disulfide nanosheets, molybdenum disulfide nanodots, molybdenum oxide nanoparticles, carbon-based molybdenum single atoms and molybdenum-based polyoxometalate nanoparticles.

2. The molybdenum-based nanocomposite material according to claim 1, characterized in that The non-molybdenum metal elements in the molybdenum-based polyoxometalate nanoparticles include any one or a combination of at least two of manganese, cobalt or bismuth.

3. The molybdenum-based nanocomposite material according to any one of claims 1 or 2, characterized in that The particle size D50 of the molybdenum-based nanocomposite material is 10-100 nm.

4. A method for preparing a molybdenum-based nanocomposite material according to any one of claims 1 to 3, characterized in that: The preparation method comprises the following steps: (1) mixing a molybdenum source and an organic solvent to obtain a dispersion; (2) subjecting the dispersion to a microwave hydrothermal reaction to obtain the molybdenum-based nanocomposite material.

5. The preparation method according to claim 4, characterized in that The molybdenum source in step (1) is ammonium tetrathiomolybdate; Preferably, the organic solvent in step (1) is N,N-dimethylformamide.

6. The preparation method according to claim 4 or 5, characterized in that The solid-to-liquid ratio of the molybdenum source and the organic solvent in step (1) is (0.006-0.012) g: (20-50) mL.

7. The preparation method according to any one of claims 4 to 6, characterized in that The temperature of the microwave hydrothermal reaction in step (2) is 150-200° C. Preferably, the microwave hydrothermal reaction time in step (2) is 12-20 hours.

8. The preparation method according to any one of claims 4 to 7, characterized in that The preparation method comprises the following steps: (1) dissolving ammonium tetrathiomolybdate in N,N-dimethylformamide and ultrasonicating for 30-60 minutes to obtain a dispersion; Wherein, the solid-liquid ratio of ammonium tetrathiomolybdate and N,N-dimethylformamide is (0.006-0.012) g: (20-50) mL; (2) transferring the dispersion into a microwave reactor, performing microwave hydrothermal reaction at 150-200° C. for 12-20 h, cooling to room temperature after the reaction, and then washing and centrifuging to obtain a precipitate, and then drying the precipitate at 40-80° C. for 4-8 h to obtain the molybdenum-based nanocomposite material.

9. A use of the molybdenum-based nanocomposite material according to any one of claims 1 to 3, characterized in that: The molybdenum-based nanocomposite material is used to improve intestinal flora disorder caused by the use of antibiotics.

10. The use according to claim 9, characterized in that The molybdenum-based nanocomposite material can be used in any one of rodents, rabbits, dogs, pigs, sheep or monkeys.

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