Nano-silver self-assembled high-efficiency disinfectant synthesized by water extract of herba epimedii stalks

Abstract

The invention relates to the fields of environmental protection, fire protection and new materials, in particular to a nano-silver self-assembled efficient disinfectant synthesized by a water extract of epimedium stems. The method comprises the following steps: weighing 10 g of epimedium stem powder, putting the epimedium stem powder into a beaker, then adding 100 mL of purified water into the beaker, putting the beaker on an electrothermal furnace, heating until boiling, then heating for 30 min, after a solid-liquid mixture is cooled, filtering impurities by using gauze, centrifuging for 10 min at a speed of 4000 r / min, retaining supernate, and fixing the volume to 100 mL; 0.17 g of silver nitrate powder is weighed and added into a beaker, then 100 mL of purified water is added for dissolution, and a silver nitrate solution is prepared; adding 20mL of the water extracting solution of the epimedium stems after constant volume into the beaker; mixing the solution, and stirring for 2 hours by using a magnetic stirrer; and the temperature is 60 DEG C to obtain the herba epimedii water extract-nano-silver self-assembled solution.

Description

Technical Field

[0001] This invention relates to the fields of environmental protection, fire protection, and new materials, and in particular to a nano-silver self-assembled high-efficiency disinfectant synthesized from the aqueous extract of Epimedium stems. Background Technology

[0002] Epimedium is a perennial herb belonging to the genus Epimedium in the family Berberidaceae. As a tonic in traditional Chinese medicine, Epimedium was first recorded in the *Shennong Bencao Jing* (Shennong's Classic of Materia Medica), boasting a history of over 2000 years. It is one of the most widely used and oldest traditional Chinese medicines. Epimedium was included in the *Chinese Pharmacopoeia* in 1963, with its medicinal parts being the stems and leaves. The 1977 edition of the *Chinese Pharmacopoeia* changed this to the aerial parts, and the 2010 edition further changed it to the dried leaves, a designation that remains in use today.

[0003] Therefore, a large amount of Epimedium stems were subsequently discarded and became waste.

[0004] On September 11, 2025, a search was conducted in the China Patent Publication Database using "Epimedium and stems and nano-silver and disinfection" as the abstract keywords and the option to allow synonym expansion was selected. No relevant literature was found.

[0005] On September 11, 2025, an abstract search was conducted on CNKI (China National Knowledge Infrastructure) using the keywords "Epimedium and stems and nano-silver and disinfection," but no relevant literature was found. Summary of the Invention

[0006] The purpose of the invention is to provide a more effective nano-silver self-assembled high-efficiency disinfectant synthesized from the aqueous extract of Epimedium stems. Specific objectives are detailed in the specific implementation section, which describes several substantial technical effects.

[0007] To achieve the above objectives, the present invention adopts the following technical solution:

[0008] A highly efficient disinfectant solution synthesized from the aqueous extract of Epimedium stems is characterized by the following steps: 10 g of Epimedium stem powder is weighed into a beaker, and 100 mL of purified water is added. The beaker is heated to boiling on an electric stove and then heated for 30 min. After the solid-liquid mixture cools, impurities are filtered through gauze, and the mixture is centrifuged at 4000 r / min for 10 min. The supernatant is retained and the volume is adjusted to 100 mL. 0.17 g of silver nitrate powder is weighed into the beaker and dissolved in 100 mL of purified water to prepare a silver nitrate solution. 20 mL of the adjusted volume of the Epimedium stem aqueous extract is added to the beaker. The solutions are mixed and stirred with a magnetic stirrer for 2 h. The solution is then heated to 60 °C to obtain the Epimedium aqueous extract-silver self-assembled solution.

[0009] A further technical solution of the present invention is that the stems of Epimedium are any one of the three varieties of Epimedium: Epimedium sagittatum, Epimedium wushanense, and Epimedium pubescens, or the stems of Epimedium harvested in a concentrated manner are naturally air-dried, crushed by a pulverizer, passed through a 100-mesh sieve, and refrigerated for later use.

[0010] A further technical solution of the present invention is that, during the process of heating to boiling and then heating for another 30 minutes, 20 mL of purified water is added in the middle to prevent it from drying out.

[0011] A further technical solution of the present invention is that the pilot-scale test of the self-assembled high-efficiency disinfectant is achieved through a dedicated self-cleaning, non-clogging reaction device;

[0012] The dedicated self-cleaning and non-clogging reaction equipment includes a reaction vessel 1, which is a reaction vessel capable of heating and stirring. A feed port 2 and a motor docking shaft 3 are arranged on the top of the reaction vessel 1.

[0013] A discharge pipe 4 is arranged at the bottom of the reactor 1;

[0014] The discharge pipe 4 is connected to the special filter separation box 5. The special filter separation box 5 has an inclined filter plate 53 arranged in the middle. The bottom of the inclined filter plate 53 is closer to one end of the discharge pipe 4.

[0015] The inclined filter plate 53 divides the interior of the special filter separation box 5 into a filter residue space 54 and a liquid space 55;

[0016] A lower discharge port 51 is arranged below the filter residue space 54;

[0017] Liquid separation pipes 52 are arranged on the side of the liquid space 55.

[0018] A further technical solution of the present invention is that the inclined filter plate 53 is a filter plate capable of filtering a 100-mesh sieve.

[0019] A further technical solution of the present invention is that the mixed liquid coming out of the discharge pipe 4 can wash away the material attached to the inclined filter plate 53 on the left side of the inclined filter plate 53.

[0020] A further technical solution of the present invention is that the lower discharge port 51 includes a discharge cone structure.

[0021] A further technical solution of the present invention is that the liquid separation pipe 52 corresponds to the finished solution.

[0022] The present invention, employing the above technical solution, has the following advantages over the prior art: Low cost: All materials are waste materials and are water extracts, resulting in low cost and a simple preparation process; Green and environmentally friendly: No toxic or harmful chemical reagents are required; synthesis can be achieved simply by heating and adding silver nitrate; Excellent performance: The prepared material, diluted 320-1280 times, exhibits significant antibacterial effects against Staphylococcus aureus, Escherichia coli, and Pseudomonas aeruginosa; Broad application prospects: It can be developed into disinfection materials for multiple fields. Attached Figure Description

[0023] To further illustrate the present invention, the following description is provided in conjunction with the accompanying drawings:

[0024] Figure 1 The antibacterial effects of aqueous extracts of Epimedium stems from different varieties and nano-silver self-assembled materials on Staphylococcus aureus, Escherichia coli, and Pseudomonas aeruginosa are shown in the figure. Figure 1, 2, and 3 show the antibacterial zones of the aqueous extract-nano-silver self-assembled composite material synthesized from the aqueous extracts of Epimedium stems from three varieties: Epimedium sagittatum, Epimedium wushanense, and Epimedium pubescens. Figure 4 shows the blank control.

[0025] Figure 2 Table 1 shows the diameter (mm) of the inhibition zone after diluting the aqueous extract of Epimedium stems and nano-silver self-assembled composite material of different varieties by 10 times; Table 2 shows the minimum MIC value (μg / mL) of the antibacterial activity of the aqueous extract of Epimedium stems and nano-silver self-assembled composite material; and Table 3 shows the dilution factor corresponding to the minimum MIC value of the antibacterial activity of the aqueous extract of Epimedium stems and nano-silver self-assembled composite material.

[0026] Figure 3 The images show TEM images of Epimedium sagittatum-silver nanoparticles at 100 nm and 50 nm, along with elemental distribution. The images reveal an irregular shape, crystalline surface features, texture, and good dispersion. The silver element is tightly bound or adsorbed by carbonaceous materials, and the material exhibits oxide and copper element signals.

[0027] Figure 4 The images show TEM images of Epimedium wushanense-silver nanoparticles at 100 nm and 50 nm, along with elemental distribution. The images reveal an irregular shape, crystalline surface features, texture, and good dispersion. The silver element is tightly bound or adsorbed by carbonaceous materials, and the material exhibits oxygen and copper signals.

[0028] Figure 5 The images show TEM images of Epimedium pubescens-silver nanoparticles at 100 nm and 50 nm, along with elemental distribution. The images reveal an irregular shape, crystalline surface features, texture, and good dispersion. The silver element is tightly bound or adsorbed by carbonaceous materials, and the material exhibits strong oxygen and copper signals.

[0029] Figure 6Energy dispersive spectroscopy and elemental ratio diagram of Epimedium sagittatum-silver nanoparticles;

[0030] Figure 7 Energy dispersive spectroscopy and elemental ratio diagram of Epimedium wushanense-nano silver;

[0031] Figure 8 Energy dispersive spectroscopy and elemental ratio diagram of Epimedium pubescens-nano silver;

[0032] Figure 9 It is a dedicated self-cleaning, non-clogging reaction device;

[0033] Figure 10 This is a structural diagram of a dedicated filter separation box;

[0034] Figure 11 This comparative table shows the results of minimum inhibitory concentrations (MICs) of antimicrobial active substances prepared by different synthetic methods against various pathogenic / conditional pathogenic bacteria. Its core purpose is to evaluate the antimicrobial efficacy of antimicrobial substances prepared under different synthetic processes, providing experimental basis for the research and development and process screening of antimicrobial materials / formulations.

[0035] The components include: 1. Reactor; 2. Feed port; 3. Motor connection shaft; 4. Discharge pipe; 5. Dedicated filter separation box; 51. Lower discharge port; 52. Liquid separation pipe; 53. Inclined filter plate; 54. Filter residue space; 55. Liquid space. Detailed Implementation

[0036] The present invention will be further illustrated below with reference to the accompanying drawings and specific embodiments. It should be understood that the following specific embodiments are for illustrative purposes only and are not intended to limit the scope of the invention. In the description of the present invention, it should be noted that the terms "center," "upper," "lower," "left," "right," "vertical," "horizontal," "inner," "outer," "top," and "bottom," etc., indicate the orientation or positional relationship based on the orientation or positional relationship shown in the accompanying drawings. They are only for the convenience of describing the present invention and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation. Therefore, they should not be construed as limitations on the present invention. In addition, unless otherwise expressly specified and limited, the terms "installed," "connected," and "linked" should be interpreted broadly. For example, they can refer to a fixed connection, a detachable connection, or an integral connection; they can refer to a mechanical connection or an electrical connection; they can refer to a direct connection or an indirect connection through an intermediate medium; and they can refer to the internal communication of two components. For those skilled in the art, the specific meaning of the above terms in the present invention can be understood according to the specific circumstances.

[0037] It should be noted that, in this document, relational terms such as "first" and "second" are used only to distinguish one entity or operation from another, and do not necessarily require or imply any such actual relationship or order between these entities or operations. Furthermore, the terms "comprising," "including," or any other variations thereof are intended to cover non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements includes not only those elements but also other elements not expressly listed, or elements inherent to such process, method, article, or apparatus.

[0038] This patent provides multiple parallel solutions; the different descriptions represent improved solutions or parallel solutions based on the basic solution. Each solution has its own unique characteristics. Furthermore, the technical features involved in the different embodiments of the invention described below can be combined with each other as long as they do not conflict with each other. Fixing methods not described herein can be any type of fixing, such as threaded fixing, bolt fixing, or adhesive bonding.

[0039] Example 1: Referring to all the accompanying drawings; a highly efficient disinfectant solution of nano-silver self-assembled from Epimedium stem aqueous extract is characterized by the following steps: 10 g of Epimedium stem powder is weighed into a beaker, and then 100 mL of purified water is added to the beaker. The beaker is heated to boiling on an electric furnace and then heated for 30 min. After the solid-liquid mixture cools, impurities are filtered through gauze, and the mixture is centrifuged at 4000 r / min for 10 min. The supernatant is retained and the volume is adjusted to 100 mL. 0.17 g of silver nitrate powder is weighed and added to the beaker, and then 100 mL of purified water is added to dissolve it, preparing a silver nitrate solution. 20 mL of the adjusted volume Epimedium stem aqueous extract is added to the beaker. The solutions are mixed and stirred with a magnetic stirrer for 2 h. The temperature is 60℃ to obtain the Epimedium aqueous extract-nano-silver self-assembled solution. The substantive technical effects and implementation process of the technical solution described herein, i.e., its basic functions, are as follows: The stems of Epimedium contain various active ingredients, such as icariin and icariin derivatives. These ingredients have reducing properties and can act as reducing agents through redox reactions to reduce silver ions in silver nitrate to elemental silver, with a particle size reaching the nanoscale. This element then participates in solution self-assembly to form a nano-silver composite material. This patent utilizes aqueous extracts from the stems of three Epimedium varieties—Epimedium sagittatum, Epimedium wushanense, and Epimedium pubescens—to prepare an aqueous extract-nano-silver self-assembled composite material. The only reagent required for this material is a 10 mM silver nitrate solution. The Epimedium stem extract is an aqueous extract, and the resulting composite material is a self-assembly system of aqueous extract-nano-silver and active ingredients. This material possesses both the properties of nano-silver and the antibacterial function of the active ingredients in the aqueous extract of Epimedium stems. The two have a synergistic effect, thus exhibiting strong antibacterial activity. It can be used as a disinfectant against common drug-resistant bacteria such as Escherichia coli and Staphylococcus aureus, as well as Pseudomonas aeruginosa, a common bacterium in wound infections. It can be developed into highly effective disinfectant preparations and products such as disinfectant material 6599, skin disinfection materials, and skin dressings.

[0040] Its antibacterial properties were found through antibacterial experiments, such as... Figure 1 As shown in Tables 1 and 2:

[0041] Table 1. Diameter of the inhibition zone (mm) after 10-fold dilution of aqueous extract of Epimedium stems and nano-silver self-assembled composite material.

[0042] the large intestine Green pus Golden grape Epimedium sagittatum nanosilver 13.75±0.07 13.35±0.21 11.55±0.07 Epimedium nanosilver from Wushan 13.45±0.07 13.55±0.21 11.70±0.14 Epimedium nanosilver 13.70±0.28 14.00±0.14 11.75±0.21

[0043] Table 2. Minimum MIC (micronized index) of antibacterial activity of Epimedium stem aqueous extract-nano-silver self-assembled composite material (μg / mL)

[0044] the large intestine Green pus Golden grape Epimedium sagittatum nanosilver 8.75 8.75 4.375 Epimedium nanosilver from Wushan 4.375 8.75 4.375 Epimedium nanosilver 4.375 4.375 2.187

[0045] Note: The concentrations in the table are equivalent concentrations calculated based on the amount of silver nitrate added.

[0046] Table 3. Dilution factors corresponding to the minimum antibacterial MIC values ​​of Epimedium stem aqueous extract-nano silver self-assembled composite material

[0047] the large intestine Green pus Golden grape Epimedium sagittatum nanosilver 320 320 640 Epimedium nanosilver from Wushan 640 320 640 Epimedium nanosilver 640 640 1280

[0048] Note: The table shows the dilution factors corresponding to the dilution of the synthesized silver nanomaterials before MIC measurement.

[0049] As shown in the table and figure above, its inhibition zone is obvious, the minimum inhibitory concentration (MIC) is lower than that of other bactericides, and the bactericidal effect is obvious. The prepared material, diluted 320-1280 times, has a significant antibacterial effect against Staphylococcus aureus, Escherichia coli, and Pseudomonas aeruginosa.

[0050] 1. Epimedium Materials: The stems of three varieties of Epimedium—Arrow-leaf Epimedium, Wushan Epimedium, and Soft-haired Epimedium—are naturally air-dried after harvesting, then crushed in a pulverizer, passed through a 100-mesh sieve, and refrigerated for later use.

[0051] 2. Preparation of nano-silver composite material: Weigh 10 g of Epimedium stem powder into a beaker, then add 100 mL of purified water. Heat the beaker to boiling point on an electric stove and continue heating for 30 min. Add another 20 mL of purified water midway to prevent drying. After the solid-liquid mixture cools, filter out impurities with gauze, centrifuge at 4000 r / min for 10 min, retain the supernatant, and dilute to 100 mL. Weigh 0.17 g of silver nitrate powder and add it to the beaker, then add 100 mL of purified water to dissolve it, preparing a silver nitrate solution. Add 20 mL of the diluted Epimedium stem aqueous extract to the beaker. Mix the solutions and stir with a magnetic stirrer for 2 h. The Epimedium aqueous extract-nano-silver self-assembled solution is obtained at 60℃.

[0052] Material characterization

[0053] TEM scanning electron microscope and elemental distribution images

[0054] Figure 3 As can be seen from the data, the material exhibits an irregular shape, crystalline surface features, texture, and good dispersion. The silver element in the material is tightly bound or adsorbed by carbonaceous materials, and it shows signs of oxides and copper elements.

[0055] Figure 4 As can be seen from the data, the material exhibits an irregular shape, crystalline surface features, texture, and good dispersion. The silver element in the material is tightly bound or adsorbed by carbonaceous materials, and it also shows signals of oxygen and copper elements.

[0056] Figure 5 As can be seen from the data, the material exhibits an irregular shape, crystalline surface features, texture, and good dispersion. The silver element in the material is tightly bound or adsorbed by carbonaceous materials, and it shows strong oxygen and copper element signals.

[0057] Technical advantages:

[0058] Low cost: All materials are waste materials and are water extracts, so the cost is low and the preparation process is simple;

[0059] Green and environmentally friendly: It requires no toxic or harmful chemical reagents; it can be synthesized simply by heating and adding silver nitrate.

[0060] Excellent performance: The prepared material, diluted 320-1280 times, has a significant antibacterial effect against Staphylococcus aureus, Escherichia coli, and Pseudomonas aeruginosa;

[0061] It has broad application prospects: it can be developed into a disinfection material for multiple fields;

[0062] Advanced technology: The nano-silver developed from Epimedium stems is unprecedented and innovative.

[0063] The stems of Epimedium are obtained from any one of the three varieties of Epimedium: Epimedium sagittatum, Epimedium wushanense, and Epimedium pubescens, or from the stems of plants harvested in a concentrated manner. After being naturally air-dried, they are crushed in a pulverizer, passed through a 100-mesh sieve, and refrigerated for later use.

[0064] During the process of heating to boiling and then heating for another 30 minutes, 20mL of purified water was added halfway through to prevent it from drying out.

[0065] Example 2: As a further possible improvement, parallel solution, or optional independent solution, combined with Figure 9 and Figure 10 The pilot-scale test of the self-assembling high-efficiency disinfectant was achieved using a dedicated self-cleaning, non-clogging reaction device.

[0066] The dedicated self-cleaning and non-clogging reaction equipment includes a reaction vessel 1, which is a reaction vessel capable of heating and stirring. A feed port 2 and a motor docking shaft 3 are arranged on the top of the reaction vessel 1.

[0067] A discharge pipe 4 is arranged at the bottom of the reactor 1;

[0068] The discharge pipe 4 is connected to the special filter separation box 5. The special filter separation box 5 has an inclined filter plate 53 arranged in the middle. The bottom of the inclined filter plate 53 is closer to one end of the discharge pipe 4.

[0069] The inclined filter plate 53 divides the interior of the special filter separation box 5 into a filter residue space 54 and a liquid space 55;

[0070] A lower discharge port 51 is arranged below the filter residue space 54;

[0071] A liquid separation pipe 52 is arranged on the side of the liquid space 55. The substantive technical effect and implementation process of this technical solution, i.e., its basic function, are as follows: The inclined filter plate 53 is a filter plate capable of filtering through a 100-mesh sieve. The mixed liquid coming out of the discharge pipe 4 can wash away the substances adhering to the inclined filter plate 53 on its left side. The lower discharge port 51 includes a discharge cone structure. The liquid separation pipe 52 corresponds to the finished solution.

[0072] This prevents substances from adhering to the inclined filter plate 53, and the impact makes it easy to clean the residue.

[0073] Innovatively, each of the above effects exists independently, yet a single structure can be used to combine the results.

[0074] The foregoing has shown and described the basic principles, main features, and advantages of the present invention. Those skilled in the art should understand that the present invention is not limited to the above embodiments. The embodiments and descriptions in the specification are merely illustrative of the principles of the invention. Various changes and modifications can be made to the invention without departing from its spirit and scope, and all such changes and modifications fall within the scope of the claims.

Claims

1. A highly efficient disinfectant solution synthesized from the aqueous extract of Epimedium stems using nano-silver self-assembly, characterized in that... Weigh 10 g of Epimedium stem powder into a beaker, then add 100 mL of purified water to the beaker. Place the beaker on an electric stove and heat to boiling, then heat for another 30 min. After the solid-liquid mixture cools, filter the impurities with gauze, centrifuge at 4000 r / min for 10 min, retain the supernatant, and bring the volume to 100 mL. Weigh 0.17 g of silver nitrate powder and add it to the beaker, then add 100 mL of purified water to dissolve it, preparing a silver nitrate solution. Add 20 mL of the Epimedium stem water extract to the beaker. Mix the solutions and stir with a magnetic stirrer for 2 h. The temperature is 60℃ to obtain the Epimedium water extract-nano silver self-assembled solution.

2. The nano-silver self-assembled high-efficiency disinfectant synthesized from the aqueous extract of Epimedium stems as described in claim 1, characterized in that, The stems of Epimedium are obtained from any one of the three varieties of Epimedium: Epimedium sagittatum, Epimedium wushanense, and Epimedium pubescens, or from the stems of plants harvested in a concentrated manner. After being naturally air-dried, they are crushed in a pulverizer, passed through a 100-mesh sieve, and refrigerated for later use.

3. The nano-silver self-assembled high-efficiency disinfectant synthesized from the aqueous extract of Epimedium stems as described in claim 1, characterized in that, During the process of heating to boiling and then heating for another 30 minutes, 20mL of purified water was added halfway through to prevent it from drying out.

4. The nano-silver self-assembled high-efficiency disinfectant synthesized from the aqueous extract of Epimedium stems as described in claim 1, characterized in that, The pilot-scale test of the self-assembled high-efficiency disinfectant was achieved using a dedicated self-cleaning, non-clogging reaction device. The dedicated self-cleaning non-clogging reaction equipment includes a reaction vessel (1), which is a reaction vessel that can be heated and stirred, and a feed port (2) and a motor docking shaft (3) are arranged on the top of the reaction vessel (1). The reactor (1) is equipped with a discharge pipe (4) at its bottom. The discharge pipe (4) is connected to the special filter separation box (5). An inclined filter plate (53) is arranged in the middle of the special filter separation box (5). The bottom of the inclined filter plate (53) is closer to one end of the discharge pipe (4). The inclined filter plate (53) divides the interior of the special filter separation box (5) into a filter cake space (54) and a liquid space (55). A lower discharge port (51) is arranged below the filter residue space (54); Liquid separation pipes (52) are arranged on the side of the liquid space (55).

5. The nano-silver self-assembled high-efficiency disinfectant synthesized from the aqueous extract of Epimedium stems as described in claim 1, characterized in that, The inclined filter plate (53) is a filter plate capable of filtering a 100-mesh sieve.

6. The nano-silver self-assembled high-efficiency disinfectant synthesized from the aqueous extract of Epimedium stems as described in claim 1, characterized in that, The mixed liquid coming out of the discharge pipe (4) can flush the material attached to the inclined filter plate (53) on the left side of the inclined filter plate (53).

7. The nano-silver self-assembled high-efficiency disinfectant synthesized from the aqueous extract of Epimedium stems as described in claim 1, characterized in that, The lower discharge port (51) includes a discharge cone structure.

8. The nano-silver self-assembled high-efficiency disinfectant synthesized from the aqueous extract of Epimedium stems as described in claim 1, characterized in that, The liquid separation pipe (52) corresponds to the finished solution.

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