Preparation method of aromatic antibacterial real silk

Abstract

The invention relates to the technical field of aromatic antibacterial materials, in particular to a preparation method of aromatic antibacterial real silk, which comprises the following steps: step 1, soaking real silk in a copper salt and PVP (Polyvinyl Pyrrolidone) aqueous solution for 15-30 minutes; step 2, adding a 2-methylimidazole aqueous solution with the same volume into the copper salt solution, reacting at room temperature for 1-2 hours, taking out the real silk, and drying to obtain Cu-MOF loaded real silk; step 3, soaking the Cu-MOF loaded real silk in an ethanol solution of essence for 2-3 hours, taking out and airing to obtain the aromatic antibacterial real silk. According to the invention, water is taken as a medium, Cu-MOF is loaded on the real silk by adopting an in-situ growth method at room temperature, and the real silk is endowed with multiple functions of fragrance, antibiosis, ultraviolet resistance and the like. The method is green and environment-friendly, and is convenient for industrial production.

Description

Technical Field

[0001] This invention relates to the field of aromatic antibacterial materials technology, and in particular to a method for preparing aromatic antibacterial silk. Background Technology

[0002] Silk, a natural protein fiber, is highly prized for its luster, feel, moisture absorption, and skin-friendliness. For silk, fragrance finishing not only enhances its added value and luxurious experience but can also be combined with health and antibacterial functions. However, silk protein fibers are susceptible to high temperatures and strong chemical environments, and their fragrances are volatile. Therefore, achieving long-lasting, slow-release fragrance finishing without damaging the fiber is a key challenge. Currently, the most mature and widely used technology is microencapsulation, which encapsulates fragrances into micron or nano-sized capsules using wall-forming materials, releasing the fragrance through physical interactions (friction, pressure) or slow-release mechanisms. Another approach is cyclodextrin inclusion complex technology, which utilizes the cyclic structure of cyclodextrin—a hydrophobic inner cavity and a hydrophilic outer wall—to "embed" fragrance molecules within the cavity through intermolecular forces, forming a stable inclusion complex that slowly releases the fragrance. In recent years, nanomaterial loading and composite finishing have become research hotspots. Fragrances are adsorbed using the high specific surface area and pore structure of porous nanomaterials (such as mesoporous silica nanoparticles, metal-organic frameworks, and cellulose nanofibers), and then applied to silk through impregnation or coating. Metal-organic frameworks, with their ultra-high porosity and tunable pore size, show great potential for fragrance loading and controlled release, and represent a cutting-edge research direction.

[0003] Copper-based metal-organic frameworks (Cu-MOFs) are open-cell framework structures with channels, formed by copper ions as nodes and organic ligands as connectors, linked by strong coordination bonds. They possess excellent properties such as high specific surface area, high porosity, and tunable porous structure, overcoming the limitations of porous materials like zeolites, activated carbon, and mesoporous silica. Although there are many reports on the preparation and application of Cu-MOFs in textiles, some problems still exist. Currently, the commonly used method for loading Cu-MOFs onto fabrics is the layer-by-layer self-assembly method. For example, patent CN202210487372.6 discloses a method for preparing antibacterial wool fabric loaded with PVP / Cu-MOFs, which loads Cu-MOF crystals onto the wool by alternately immersing it in metal and ligand solutions. While this method can increase the crystal loading on the wool, the preparation process is frequent and costly, hindering industrial production.

[0004] With the continuous development of industry, low-cost and environmentally friendly preparation processes are receiving increasing attention. However, most metal-organic frameworks (MOFs) currently use polluting organic solvents for their preparation. For example, patent CN201811529778.6 discloses a method for preparing MOFs based on fabric carriers, which grows crystals on a fiber substrate using a solvothermal method and employs various harmful solvents, which is detrimental to the development of green and environmentally friendly practices.

[0005] To address the aforementioned issues, this application proposes a green and environmentally friendly method for preparing aromatic antibacterial silk. Summary of the Invention

[0006] The purpose of this invention is to overcome the shortcomings of existing technologies by proposing a method for preparing aromatic antibacterial silk. The method involves immersing silk in an aqueous solution of copper salts containing PVP for 15-30 minutes, then slowly adding an equal volume of 2-methylimidazole aqueous solution to the copper salt solution. The reaction is carried out at room temperature for 1-2 hours. The silk is then removed, dried, and the resulting Cu-MOF-loaded silk is obtained. The Cu-MOF-loaded silk is then immersed in an ethanol solution of fragrance for 2-3 hours, removed, and air-dried to obtain aromatic antibacterial silk. This method is convenient, environmentally friendly, and suitable for industrial production.

[0007] To achieve the above objectives, the present invention adopts the following technical solution: a method for preparing aromatic antibacterial silk, the specific steps of which are as follows:

[0008] Step 1: Immerse the silk in a copper salt and PVP aqueous solution for 15-30 minutes;

[0009] Step 2: Slowly add an equal volume of 2-methylimidazole aqueous solution to the copper salt solution, react at room temperature for 1-2 hours, remove the silk, dry it, and obtain the loaded Cu-MOF silk.

[0010] Step 3: Immerse the Cu-MOF-loaded silk in an ethanol solution of fragrance for 2-3 hours, then remove and air dry to obtain aromatic antibacterial silk.

[0011] Preferably, in step 1, the copper salt is one of copper sulfate, copper nitrate, and copper chloride, with a concentration of 0.1-0.2 mol / L; the PVP concentration is 30 g / L; and the bath ratio of silk to the copper salt and PVP aqueous solution is 1:20-1:30.

[0012] Preferably, in step 2, the concentration of 2-methylimidazole is 0.1-0.2 mol / L; and the drying temperature is 60-70℃.

[0013] Preferably, in step 3, the volume ratio of fragrance to ethanol is 1:50-1:100, and the bath ratio of silk to the ethanol solution of fragrance is 1:10-1:50.

[0014] Preferably, the silk is a silk fabric, a nonwoven fabric, or a thread.

[0015] By employing the above technical solution: firstly, Cu-MOF is rapidly and uniformly loaded onto silk using an in-situ growth method at room temperature with water as the medium. Then, by utilizing the adsorption and encapsulation effects of Cu-MOF on fragrances, as well as its antibacterial and anti-UV properties, an aromatic and antibacterial silk is produced. This method is green and environmentally friendly, operates under mild conditions, and is suitable for industrial production.

[0016] Compared with the prior art, the present invention has the following beneficial effects:

[0017] 1. The solutions involved in this invention all use water as a solvent, which is inexpensive to prepare and environmentally friendly.

[0018] 2. This invention loads Cu-MOF onto silk, which can not only encapsulate fragrance and delay its release, but also endow silk with functions such as antibacterial and anti-ultraviolet properties, and has broad application prospects.

[0019] 3. This invention has the advantages of simple equipment and convenient operation, which facilitates industrial production. Attached Figure Description

[0020] Figure 1 This is a flowchart illustrating the preparation process of the present invention. Detailed Implementation

[0021] The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings, so that those skilled in the art can better understand the advantages and features of the present invention, thereby making a clearer definition of the scope of protection of the present invention. The embodiments described in this invention are only some embodiments of the present invention, not all embodiments. All other embodiments obtained by those skilled in the art based on the embodiments of the present invention without creative effort are within the scope of protection of the present invention.

[0022] Example 1:

[0023] Reference Figure 1 A method for preparing aromatic antibacterial silk, the specific steps of which are as follows:

[0024] Step 1: Immerse the silk fabric in a 0.1 mol / L copper chloride and 30 g / L PVP aqueous solution at a bath ratio of 1:20 for 15 min;

[0025] Step 2: Slowly add an equal volume of 0.1 mol / L 2-methylimidazole aqueous solution to the copper salt solution, react at room temperature for 1 h, remove the silk fabric, dry at 60 °C to obtain Cu-MOF loaded silk fabric;

[0026] Step 3: Immerse the Cu-MOF-loaded silk fabric in a fragrance ethanol solution with a volume ratio of 1:10 at a bath ratio of 1:100 for 2 hours, then remove and air dry to obtain aromatic antibacterial silk.

[0027] Results of this embodiment: A 10cm × 10cm sample and a blank sample were placed at room temperature, and the intensity of the released fragrance was periodically measured. The fragrance retention effect of the sample under natural placement is shown in Table 1. The antibacterial rate of the prepared silk fabric against Escherichia coli and Staphylococcus aureus was measured according to GB / T 20944.3-2008 "Evaluation of Antibacterial Properties of Textiles Part 3: Shaking Method" and is shown in Table 2. The UV protection performance of the prepared multifunctional cotton fabric was measured according to GB / T 18830-2009 "Evaluation of UV Protection Performance of Textiles" and is shown in Table 3.

[0028] Example 2:

[0029] Reference Figure 1 A method for preparing aromatic antibacterial silk, the specific steps of which are as follows:

[0030] Step 1: Immerse the silk fabric in a 0.15mol / L copper sulfate and 30g / L PVP aqueous solution at a bath ratio of 1:30 for 30 minutes;

[0031] Step 2: Slowly add the same volume of 0.15 mol / L 2-methylimidazole aqueous solution to the copper salt solution, react at room temperature for 1.5 h, take out the silk fabric, dry at 60 °C to obtain Cu-MOF loaded silk fabric;

[0032] Step 3: Immerse the Cu-MOF-loaded silk fabric in a fragrance ethanol solution with a volume ratio of 1:80 at a bath ratio of 1:30 for 2 hours, remove and air dry to obtain aromatic antibacterial silk.

[0033] Results of this embodiment: A 10cm × 10cm sample and a blank sample were placed at room temperature, and the intensity of the released fragrance was periodically measured. The fragrance retention effect of the sample under natural placement is shown in Table 1. The antibacterial rate of the prepared silk fabric against Escherichia coli and Staphylococcus aureus was measured according to GB / T 20944.3-2008 "Evaluation of Antibacterial Properties of Textiles Part 3: Shaking Method" and is shown in Table 2. The UV protection performance of the prepared multifunctional cotton fabric was measured according to GB / T 18830-2009 "Evaluation of UV Protection Performance of Textiles" and is shown in Table 3.

[0034] Example 3:

[0035] Reference Figure 1 A method for preparing aromatic antibacterial silk, the specific steps of which are as follows:

[0036] Step 1: Immerse the silk fabric in a 0.2mol / L copper nitrate and 30g / L PVP aqueous solution at a bath ratio of 1:30 for 30 minutes;

[0037] Step 2: Slowly add an equal volume of 0.2 mol / L 2-methylimidazole aqueous solution to the copper salt solution, react at room temperature for 3 h, remove the silk fabric, dry at 70 °C to obtain Cu-MOF loaded silk fabric;

[0038] Step 3: Immerse the Cu-MOF-loaded silk fabric in a fragrance ethanol solution with a volume ratio of 1:50 at a bath ratio of 1:50 for 3 hours, remove and air dry to obtain aromatic antibacterial silk.

[0039] Results of this embodiment: A 10cm × 10cm sample and a blank sample were placed at room temperature, and the intensity of the released fragrance was periodically measured. The fragrance retention effect of the sample under natural placement is shown in Table 1. The antibacterial rate of the prepared silk fabric against Escherichia coli and Staphylococcus aureus was measured according to GB / T 20944.3-2008 "Evaluation of Antibacterial Properties of Textiles Part 3: Shaking Method" and is shown in Table 2. The UV protection performance of the prepared multifunctional cotton fabric was measured according to GB / T 18830-2009 "Evaluation of UV Protection Performance of Textiles" and is shown in Table 3.

[0040] Table 1. Fragrance retention effect of the sample from the examples.

[0041]

[0042] Table 2 Antibacterial rate of the samples in the examples

[0043]

[0044] Table 3 UV protection performance of the samples in the examples

[0045]

[0046] In summary, this invention first uses water as a medium to rapidly and uniformly load Cu-MOF onto silk at room temperature via an in-situ growth method. Then, utilizing the fragrance adsorption and encapsulation effects of Cu-MOF, as well as its antibacterial and anti-UV properties, a fragrant and antibacterial silk is produced. This method is environmentally friendly, operates under mild conditions, and is suitable for industrial production. The resulting multifunctional silk has promising application prospects.

[0047] The descriptions and practices disclosed in this invention are readily apparent and understandable to those skilled in the art, and various modifications and refinements can be made without departing from the principles of this invention. Therefore, any modifications or improvements made without departing from the spirit of this invention should also be considered within the scope of protection of this invention.

Claims

1. A method for preparing aromatic antibacterial silk, characterized in that, Includes the following steps: Step 1: Immerse the silk in a copper salt and PVP aqueous solution for 15-30 minutes; Step 2: Slowly add an equal volume of 2-methylimidazole aqueous solution to the copper salt solution, react at room temperature for 1-2 h, remove the silk, dry it, and obtain the loaded Cu-MOF silk. Step 3: Immerse the Cu-MOF-loaded silk in an ethanol solution of fragrance for 2-3 hours, then remove and air dry to obtain aromatic antibacterial silk.

2. The method for preparing aromatic antibacterial silk according to claim 1, characterized in that, In step 1, the copper salt is one of copper sulfate, copper nitrate, and copper chloride, with a concentration of 0.1-0.2 mol / L; the PVP concentration is 30 g / L; and the bath ratio of silk to the copper salt and PVP aqueous solution is 1:20-1:

30.

3. The method for preparing aromatic antibacterial silk according to claim 1, characterized in that, In step 2, the concentration of 2-methylimidazole is 0.1-0.2 mol / L; the drying temperature is 60-70℃.

4. The method for preparing aromatic antibacterial silk according to claim 1, characterized in that, In step 3, the volume ratio of fragrance to ethanol is 1:50-1:100, and the bath ratio of silk to ethanol solution of fragrance is 1:10-1:

50.

5. The method for preparing aromatic antibacterial silk according to claim 1, characterized in that, The silk refers to silk fabrics, non-woven fabrics, and silk threads.

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