A nanomaterial PEI-MQD with bactericidal effect

Abstract

This invention provides a novel nanomaterial, PEI-MQD, made from titanium carbide Ti3C2MXene multilayer nanosheets. This material exhibits significant bactericidal and antifungal effects against a variety of pathogenic oomycetes and fungi, including Phytophthora capsici, Phytophthora caerulea, Pythium rotundum, Phytophthora litchii, Botrytis cinerea, and Fusarium oxysporum. It can be used to control oomycete and fungal diseases in crops. Furthermore, this nanomaterial has a small particle size of 4.886±0.528nm and good biocompatibility, suggesting its potential for development into new pesticides or adjuvants.

Description

Technical Field

[0001] The present invention belongs to the research and application field of crop disease prevention and control in the subject of agronomy and plant protection, and specifically relates to a novel nanomaterial PEI-MQD with a bactericidal effect. Background Art

[0002] my country is a major agricultural producer, but crop oomycete and fungal diseases pose a serious threat to agricultural production safety, often resulting in significant economic losses. Currently, the most widely used and effective method for crop disease control is spraying chemical pesticides. However, the long-term and extensive use of chemical pesticides has led to increasingly prominent problems such as pathogen resistance, pesticide residues, and environmental pollution. This is detrimental to the sustainable development of modern agriculture and the promotion of ecological progress. There is an urgent need to develop new products for agricultural production. For years, scientists have been exploring various disease control methods. On January 29, 2022, the Ministry of Agriculture and Rural Affairs, in conjunction with relevant state departments, issued and implemented the "14th Five-Year Plan for the Development of the National Pesticide Industry," which explicitly encourages the innovative application of nanotechnology in pesticide research and development. To date, no nanomaterials exist for the control of oomycete diseases.

[0003] Pathogenic oomycetes grow and reproduce very rapidly, forming large colonies in a short period of time, causing devastating damage. Their short infection cycle also allows for widespread epidemics and outbreaks, making them difficult to control. Furthermore, the limited availability of conventional oomycetic agents and their long-term, heavy use have led to increasingly prominent problems such as pathogen resistance, pesticide residues, and environmental pollution. Summary of the Invention

[0004] The purpose of this section is to summarize some aspects of the embodiments of the present invention and briefly introduce some preferred embodiments. Some simplifications or omissions may be made in this section and the abstract and title of this application to avoid obscuring the purpose of this section, the abstract and the title of the invention, and such simplifications or omissions should not be used to limit the scope of the present invention.

[0005] In view of the above problems and / or the problems existing in the prior art, the present invention is proposed.

[0006] Therefore, the purpose of the present invention is to overcome the deficiencies in the prior art and provide a nanomaterial PEI-MQD with a bactericidal effect, characterized in that it comprises:

[0007] Its main components include titanium carbide MXene multilayer nanosheets and polyethylene diamine.

[0008] In order to solve the above technical problems, the present invention provides the following technical solutions: a method for preparing a nanomaterial PEI-MQD nanomaterial with a bactericidal effect, characterized in that:

[0009] The bactericidal nanomaterial PEI-MQD is prepared by the oxygen-free hydrothermal reaction of titanium carbide MXene multilayer nanosheets and polyethylene diamine.

[0010] As a preferred embodiment of the preparation method of the present invention, the method first uses titanium carbide Ti3C2MXene multilayer nanosheets and polyethylene diamine to undergo an anaerobic hydrothermal reaction in a reactor, and obtains the nanomaterial PEI-MQD after 3500Da dialysis interception.

[0011] As a preferred embodiment of the preparation method of the present invention, the mass ratio of titanium carbide nanosheets to polyethylene diamine in the preparation method is 2:1.

[0012] As a preferred embodiment of the preparation method of the present invention, the anaerobic hydrothermal reaction in the preparation method is an anaerobic hydrothermal reaction at 120° C. in a reactor for 8 hours.

[0013] Another object of the present invention is to overcome the deficiencies in the prior art and provide an application of a nanomaterial PEI-MQD, characterized in that the nanomaterial is used in the prevention and control of oomycete diseases.

[0014] Beneficial effects of the present invention:

[0015] The nanomaterial PEI-MQD can effectively inhibit the mycelial growth of four oomycetes (Phytophthora capsici, Phytophthora caerulea, Pythium rotundum, and Phytophthora litchii) and two fungi (Botrytis cinerea and Fusarium oxysporum). -1 There is an obvious antibacterial effect when the concentration reaches 100 mg·L -1 The nanomaterial can completely inhibit the growth of the aforementioned pathogens and has the potential to be developed into a broad-spectrum fungicide. Furthermore, the nanomaterial's small particle size allows it to be combined with other pesticides to enhance their efficacy, potentially alleviating environmental pollution and pesticide residues, and contributing to the safe production and sustainable development of modern agriculture. BRIEF DESCRIPTION OF THE DRAWINGS

[0016] In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the following briefly introduces the drawings required for describing the embodiments. Obviously, the drawings described below are only some embodiments of the present invention. Those skilled in the art can also derive other drawings based on these drawings without inventive effort. Among them:

[0017] Figure 1 Two-dimensional structure of Ti3C2 MXene; A: Scanning electron microscope photo of Ti3C2 MXene; B: XRD diffraction pattern.

[0018] Figure 2Characterization diagram of PEI-MQD; A: nanoparticles; B: zeta potential of nanoparticles; C: nanometer size under electron microscope; D: emission spectrum of nanoparticles; E: XRD diffraction pattern of nanoparticles; F: infrared absorption spectrum of nanoparticles.

[0019] Figure 3 PEI-MQD inhibits the growth of four oomycetes: the control at the top of the picture represents the control without PEI-MQD, and the remaining labels are the final nanometer concentrations in the test tube; for easy observation, the mycelium was stained with trypan blue, and the darker the color, the more mycelium there is.

[0020] Figure 4 PEI-MQD inhibits the growth of Botrytis cinerea and Fusarium oxysporum: The control at the top of the image represents a control without PEI-MQD, and the remaining labels indicate the final nanometer concentration in the test tube; for easy observation, the mycelium was stained with trypan blue; darker colors indicate more mycelium. DETAILED DESCRIPTION

[0021] In order to make the above-mentioned objects, features and advantages of the present invention more obvious and easy to understand, the specific implementation methods of the present invention are described in detail below in conjunction with the embodiments of the specification.

[0022] In the following description, many specific details are set forth to facilitate a full understanding of the present invention. However, the present invention may also be implemented in other ways different from those described herein. Those skilled in the art may make similar generalizations without violating the connotation of the present invention. Therefore, the present invention is not limited to the specific embodiments disclosed below.

[0023] Secondly, the term "one embodiment" or "embodiment" herein refers to a specific feature, structure, or characteristic that may be included in at least one implementation of the present invention. The phrase "in one embodiment" appearing in various places throughout this specification does not necessarily refer to the same embodiment, nor does it refer to a separate or selective embodiment that is mutually exclusive of other embodiments.

[0024] Example 1

[0025] 1. Disperse 50mg of Ti3C2 MXene powder in 10mL of ultrapure water and add 25mg of polyethylene diamine (molecular weight: 1800). Add the polyethylene diamine first, then the Ti3C2 MXene powder, and finally the ultrapure water. The polyethylene diamine can be added directly to the bottom of the 25mL reactor lining.

[0026] 2. N2 was introduced into the obtained dispersion for 5 minutes to remove excess oxygen in the solution and ensure that the hydrothermal reaction occurred in an oxygen-free environment as much as possible;

[0027] 3. Heat the reactor in an oven at 120°C for 8 hours, then cool to room temperature before proceeding with other operations.

[0028] 4. The solution was then placed in a centrifuge tube and allowed to stand for 1 hour. The solution was centrifuged at 5000 rpm for 5 minutes to remove the precipitate in the solution to avoid aspiration of the precipitate. 3M HCl was then added to the supernatant to adjust the pH of the reaction solution to 7.

[0029] 5. Use a dialysis bag with a molecular cutoff of 3500Da to dialyze the sample in pure water for 24 hours, changing the water every 12 hours. The final product is freeze-dried and its concentration is calculated.

[0030] The volume dialyzed is approximately twice the volume of the liquid before dialysis, and the concentration is the ratio of the mass difference of the centrifuge tube before and after freeze-drying to the volume of pure water added;

[0031] 6. Characterize nanomaterials using electron microscopy (SEM, TEM), X-ray diffraction, infrared spectroscopy, etc.

[0032] Example 2

[0033] 1. Inoculate pepper phytophthora, caerulea, phytophthora involuta, and litchi peronophthora on 10% V8 solid plates, and gray mold and Fusarium oxysporum on PDA medium, and culture in a 25°C incubator in the dark for 5-8 days;

[0034] 2. Use a sterile punch to punch holes at the edge of the freshly cultured colony, take 5 mycelial blocks (5 mm in diameter) and place them in a sterile glass test tube, add 500 μL of 10% V8 culture medium, and add 7 μL, 16 μL, 27 μL, 78 μL, and 155 μL of the nanomaterial PEI-MQD mother solution (2110 mg·L) respectively. -1 ), and the final concentrations of PEI-MQD in the culture medium were diluted with sterile water to 25, 50, 100, 250, and 500 mg·L -1 , the negative control was filled with sterile water without adding PEI-MQD, and the glass tube was placed in a 25℃ constant temperature box and cultured in the dark for 3 days;

[0035] 3. Observe the growth of mycelium and add 200 μL of trypan blue staining solution to the glass test tube. Replace it with sterile water after 1-3 hours and take photos with a camera.

[0036] It should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention and are not intended to limit the present invention. Although the present invention has been described in detail with reference to the preferred embodiments, those skilled in the art should understand that the technical solutions of the present invention may be modified or replaced by equivalents without departing from the spirit and scope of the technical solutions of the present invention, which should all be included in the scope of the claims of the present invention.

Claims

1. Application of a nanomaterial PEI-MQD with bactericidal effect in preventing and controlling oomycete diseases, characterized in that: include, The nanomaterial PEI-MQD with bactericidal effect is made of titanium carbide MXene multilayer nanosheets and polyethylene diamine; The nanomaterial PEI-MQD can effectively inhibit the mycelial growth of four oomycetes, namely, Phytophthora capsici, Phytophthora caerulea, Pythium rotundum, and Phytophthora litchii, and two fungi, namely, Botrytis cinerea and Fusarium oxysporum. -1 There is an obvious antibacterial effect when the concentration reaches 100 mg·L -1 It can completely inhibit the growth of the above pathogens.

2. The use according to claim 1, characterized in that: The preparation method of the nano material is: First, titanium carbide T i3 C2MXene multilayer nanosheets and polyethylene diamine were subjected to anaerobic hydrothermal reaction in a reactor, and the nanomaterial PEI-MQD was obtained after 3500Da dialysis interception.

3. The use according to claim 2, characterized in that: The mass ratio of the titanium carbide nanosheets to polyethylene diamine is 2:

1.

4. The use according to claim 2, wherein: The anaerobic hydrothermal reaction is carried out in a reactor at 120° C. for 8 hours.

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