Fabric antibacterial function modifier and preparation method thereof

Abstract

The invention relates to the research category of fabric modifiers, in particular to a fabric antibacterial function modifier and a preparation method thereof. The preparation method comprises the following specific preparation steps: S1, synthesizing o-vanillin o-methoxyaniline Schiff base; s2, synthesizing an o-vanillin Schiff base nickel complex; and S3, preparing the antibacterial microcapsule modifier. The prepared microcapsule is introduced to a textile through dipping, rolling and baking, spraying and other methods, and the antibacterial fabric is obtained. The antibacterial rate of the fabric modifier to escherichia coli and staphylococcus aureus reaches 99% or above, the antibacterial function is remarkably enhanced, and the antibacterial action time is long. And the preparation process is simple, controllable, low in production cost and suitable for popularization and application.

Description

Technical Field

[0001] The invention relates to the research scope of fabric modifiers, and in particular to a fabric antibacterial function modifier and a preparation method thereof. Background Art

[0002] Common textile materials are mainly divided into synthetic fibers, natural cellulose fibers and natural protein fibers. Antimicrobial agents for fabrics usually achieve their antibacterial effects by destroying bacterial cell membranes, inhibiting metabolism or denaturing or precipitating proteins in bacteria. Currently reported antimicrobial agents can be mainly divided into three types: organic antimicrobial agents, inorganic antimicrobial agents and natural antimicrobial agents. Inorganic antimicrobial agents have a wide antibacterial range and good heat resistance, but they have the disadvantages of large dosage and easy discoloration of fabrics; organic antimicrobial agents have strong antibacterial effects, but poor heat resistance and easy to produce drug resistance; natural antimicrobial agents are safe and non-toxic, and have abundant resources, but are difficult to extract.

[0003] CN110627828 A discloses a quaternary ammonium salt of organosilicon for improving antibacterial properties. The quaternary ammonium salt has the disadvantages of poor compatibility with anionic additives, easy discoloration of fabrics, and poor heat resistance. In the current existing antibacterial function modification technology, most of the modifiers used have toxic effects on human body and environment, or the modification process is complicated, affecting the feel of the fabric, so the development of new antibacterial function modifiers for fabrics is still a topic worth exploring. Summary of the invention

[0004] In view of the problems existing in the background technology, the present invention provides a fabric antibacterial function modifier and a preparation method thereof. The preparation process of the modifier is simple and the antibacterial function is strong.

[0005] To achieve the above object, the present invention provides a fabric antibacterial function modifier and a preparation method thereof comprising the following steps:

[0006] (1) Synthesis of o-vanillin condensed o-anisidine Schiff base;

[0007] (2) Synthesis of o-vanillin Schiff base nickel complex;

[0008] (3) Preparation of antibacterial microcapsule modifiers.

[0009] In the above-mentioned fabric antibacterial function modifier and its preparation method, the synthesis steps of o-vanillin condensed o-aniline Schiff base are: dissolving o-vanillin and o-aniline in anhydrous ethanol, after the reaction is completed at room temperature, removing the solvent to obtain an orange solid, and then recrystallizing to obtain a reaction product.

[0010] Preferably, the solution selected for recrystallization is ethanol.

[0011] In the above-mentioned fabric antibacterial function modifier and preparation method thereof, the synthesis steps of the o-vanillin Schiff base nickel complex are: dissolving nickel sulfate hexahydrate in anhydrous methanol and dissolving o-vanillin Schiff base in chloroform. First, the chloroform solution of o-vanillin Schiff base is placed at the bottom of a test tube, then an appropriate amount of triethylamine is added, and finally a methanol solution of nickel sulfate is added, and the o-vanillin Schiff base nickel complex is obtained by standing.

[0012]

[0013] In the above-mentioned fabric antibacterial function modifier and preparation method thereof, the steps of preparing the antibacterial microcapsule modifier are as follows: adding the o-vanillin Schiff base nickel complex to deionized water to fully dissolve, forming an emulsion by ultrasonic treatment, subjecting the emulsion to high-pressure homogenization treatment, and using a high-pressure micro-water mist nozzle to high-pressure spray molding. The spray-formed microcapsules are dried to obtain the antibacterial microcapsule modifier.

[0014] Preferably, the homogenization conditions are room temperature and pressure of 35 to 45 MPa.

[0015] Preferably, the spray drying conditions are an inlet air temperature of 180-200°C and an outlet air temperature of 80-100°C.

[0016] The prepared microcapsules are introduced onto textiles by dipping, rolling baking, spraying and the like to obtain antibacterial fabrics.

[0017] Compared with the prior art, the present invention has the following beneficial effects:

[0018] (1) The fabric antibacterial function modifier provided by the present invention has no irritating odor and can be applied to fabrics without any obstacles.

[0019] (2) The antibacterial function modifier of the fabric improves the binding degree between the antibacterial agent and the fabric fiber, which can effectively inhibit the growth of Escherichia coli and Staphylococcus aureus and greatly prolong the antibacterial action time.

[0020] (3) The preparation process of the fabric antibacterial functional modifier is simple and controllable, with low production cost, and is suitable for popular application. DETAILED DESCRIPTION

[0021] The following embodiments of the technical solution of the present invention are described in detail in conjunction with the embodiments. The following embodiments are only used to more clearly illustrate the technical solution of the present invention, and are therefore only used as examples, and cannot be used to limit the protection scope of the present invention.

[0022] It should be noted that the experimental methods used in the implementation examples are all conventional methods unless otherwise specified; the materials, reagents, etc. used, unless otherwise specified, can be obtained from commercial channels.

[0023] In the present invention, unless otherwise specified, the numerical range "a-b" represents an abbreviation of any real number combination between a-b, where a and b are real numbers. For example, the numerical range "0-5" means that all real numbers between "0-5" are listed in this document, and "0-5" is just an abbreviation of these numerical combinations.

[0024] In the present invention, unless otherwise specified, all embodiments and preferred embodiments mentioned herein can be combined with each other to form a new technical solution.

[0025] In the present invention, unless otherwise specified, all the steps mentioned herein may be performed sequentially or randomly, but are preferably performed sequentially; for example, the method includes steps (a) and (b), which means that the method may include steps (a) and (b) performed sequentially, or may include steps (b) and (a) performed sequentially; for example, the method may further include step (c), which means that step (c) may be added to the method in any order, for example, the method may include steps (a), (b) and (c), or may include steps (a), (c) and (b), or may include steps (c), (a) and (b), etc.

[0026] Example 1

[0027] 1. Weigh 6g of o-vanillin and 4.5mL of o-anisidine into a 250mL three-necked flask, add 100mL of anhydrous ethanol, stir until completely dissolved, and react at room temperature until the end point. Remove the solvent to obtain an orange solid, which is recrystallized from ethanol to obtain an orange crystalline o-vanillin condensed o-anisidine Schiff base.

[0028] 2. Weigh 0.2g NiSO4·6H2O and dissolve it in anhydrous methanol. Then weigh 0.3g o-vanillin Schiff base and dissolve it in chloroform. First place the chloroform solution with dissolved ligand at the bottom of the test tube. Then add an appropriate amount of triethylamine. Finally, add the methanol solution of nickel sulfate. Let it stand for 5 days to obtain the o-vanillin Schiff base nickel complex.

[0029] 3. Add the o-vanillin Schiff base nickel complex to deionized water to fully dissolve, form an emulsion by ultrasonic treatment, homogenize the emulsion at 45 MPa, and use a high-pressure micro-water mist nozzle to perform high-pressure spray molding. Dry the spray-formed microcapsules to obtain an antibacterial microcapsule modifier.

[0030] Example 2

[0031] 1. Weigh 6g of o-vanillin and 4.5mL of o-anisidine into a 250mL three-necked flask, add 100mL of anhydrous ethanol, stir until completely dissolved, and react at room temperature until the end point. Remove the solvent to obtain an orange solid, which is recrystallized from ethanol to obtain an orange crystalline o-vanillin condensed o-anisidine Schiff base.

[0032] 2. Weigh 0.2g NiSO4·6H2O and dissolve it in anhydrous methanol. Then weigh 0.3g o-vanillin Schiff base and dissolve it in chloroform. First place the chloroform solution with dissolved ligand at the bottom of the test tube. Then add an appropriate amount of triethylamine. Finally, add the methanol solution of nickel sulfate. Let it stand for 6 days to obtain the o-vanillin Schiff base nickel complex.

[0033] The nickel complex of o-vanillin Schiff base is added to deionized water and fully dissolved, an emulsion is formed by ultrasonic treatment, the emulsion is subjected to 40MPa high-pressure homogenization treatment, and a high-pressure micro-water mist nozzle is used to perform high-pressure spray molding. The spray-formed microcapsules are dried to obtain an antibacterial microcapsule modifier.

[0034] Example 3

[0035] 1. Weigh 3g of o-vanillin and 2.3mL of o-anisidine into a 250mL three-necked flask, add 50mL of anhydrous ethanol, stir until completely dissolved, and react at room temperature until the end point. Remove the solvent to obtain an orange solid, which is recrystallized from ethanol to obtain an orange crystalline o-vanillin condensed o-anisidine Schiff base.

[0036] 2. Weigh 0.2g NiSO4·6H2O and dissolve it in anhydrous methanol. Then weigh 0.3g o-vanillin Schiff base and dissolve it in chloroform. First place the chloroform solution with dissolved ligand at the bottom of the test tube. Then add an appropriate amount of triethylamine. Finally, add the methanol solution of nickel sulfate. Let it stand for 5 days to obtain the o-vanillin Schiff base nickel complex.

[0037] The o-vanillin Schiff base nickel complex is added to deionized water and fully dissolved, an emulsion is formed by ultrasonic treatment, the emulsion is subjected to 45MPa high-pressure homogenization treatment, and a high-pressure micro-water mist nozzle is used to perform high-pressure spray molding. The spray-formed microcapsules are dried to obtain an antibacterial microcapsule modifier.

[0038] Example 4

[0039] 1. Weigh 3g of o-vanillin and 2.3mL of o-anisidine into a 250mL three-necked flask, add 50mL of anhydrous ethanol, stir until completely dissolved, and react at room temperature until the end point. Remove the solvent to obtain an orange solid, which is recrystallized from ethanol to obtain an orange crystalline o-vanillin condensed o-anisidine Schiff base.

[0040] 2. Weigh 0.2g NiSO4·6H2O and dissolve it in anhydrous methanol. Then weigh 0.3g o-vanillin Schiff base and dissolve it in chloroform. First place the chloroform solution with dissolved ligand at the bottom of the test tube. Then add an appropriate amount of triethylamine. Finally, add the methanol solution of nickel sulfate. Let it stand for 7 days to obtain the o-vanillin Schiff base nickel complex.

[0041] The o-vanillin Schiff base nickel complex is added to deionized water and fully dissolved, an emulsion is formed by ultrasonic treatment, the emulsion is subjected to 30 MPa high-pressure homogenization treatment, and a high-pressure micro-water mist nozzle is used to perform high-pressure spray molding. The spray-formed microcapsules are dried to obtain an antibacterial microcapsule modifier.

[0042] Antibacterial performance test

[0043] According to GB / T 20944.3-2008 “Evaluation of antibacterial properties of textiles Part 3: Oscillation method”, Escherichia coli and Staph ylococcus aureus were used to evaluate the antibacterial effect of cotton fabrics.

[0044] The experimental group used cotton fabrics treated with antibacterial functional modifiers, and the control group used cotton fabrics without any treatment.

[0045] First, a single colony on the agar plate was inoculated into a conical flask containing 20 mL of nutrient broth and cultured at 37 °C for 24 h to a bacterial concentration of 1 × 10 9 ~5×10 9 The sterilized test fiber and 70 mL of PBS solution were mixed in a 250 mL conical flask, and 5 mL of diluted bacterial solution (3×10 5 ~4×10 5 CFU / mL). The conical flask was sealed and placed in a constant temperature shaking incubator at 150 rpm and cultured at 24°C for 18 hours. Subsequently, the bacterial solution in contact with the test fabric sample was diluted to an appropriate multiple using a sterilized PBS solution and inoculated into an agar medium and cultured in a constant temperature shaking incubator at 37°C for 24 hours. Finally, the culture medium with a colony count of 30 to 300 CFU was counted and recorded. Similarly, this method was used to test Staphylococcus aureus. The final results are shown in Table 1.

[0046] The inhibition rate was calculated using the following formula:

[0047] Antibacterial rate (%) = (N c -N S ) / N C ×100

[0048] Nc: number of colonies on standard cotton fabric culture medium; NS: number of colonies on test sample culture medium

[0049] Table 1

[0050]

[0051] The above results show that the antibacterial rate of the cotton fabric treated with the antibacterial modifier provided by the present invention against Staphylococcus aureus and Escherichia coli is significantly improved compared with the untreated cotton fabric.

[0052] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention, rather than to limit it. Although the present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that they can still modify the technical solutions described in the aforementioned embodiments, or replace some or all of the technical features therein by equivalents. However, these modifications or replacements do not cause the essence of the corresponding technical solutions to deviate from the scope of the technical solutions of the embodiments of the present invention.

Claims

1. A fabric antibacterial function modifier and a preparation method thereof, comprising the following steps: (1) Synthesis of o-vanillin condensed o-anisidine Schiff base; (2) Synthesis of o-vanillin Schiff base nickel complex; (3) Preparation of antibacterial microcapsule modifiers.

2. A fabric antibacterial function modifier and a preparation method thereof according to claim 1, characterized in that: The synthesis steps of the o-vanillin condensed o-aniline Schiff base are as follows: o-vanillin and o-aniline are dissolved in anhydrous ethanol, after the reaction is completed at room temperature, the solvent is removed to obtain an orange solid, and then the reaction product is obtained by recrystallization.

3. A fabric antibacterial function modifier and a preparation method thereof according to claim 2, characterized in that: The solution used for recrystallization is ethanol.

4. A fabric antibacterial function modifier and a preparation method thereof according to claim 1, characterized in that: The synthesis steps of the o-vanillin Schiff base nickel complex are as follows: nickel sulfate hexahydrate is dissolved in anhydrous methanol, and o-vanillin Schiff base is dissolved in chloroform. The chloroform solution of o-vanillin Schiff base is first placed at the bottom of a test tube, then an appropriate amount of triethylamine is added, and finally a methanol solution of nickel sulfate is added, and the o-vanillin Schiff base nickel complex is obtained by standing.

5. A fabric antibacterial function modifier and a preparation method thereof according to claim 1, characterized in that: The steps of preparing the antibacterial microcapsule modifier are as follows: adding the o-vanillin Schiff base nickel complex to deionized water to fully dissolve it, forming an emulsion by ultrasonic treatment, performing high-pressure homogenization treatment on the emulsion, using a high-pressure micro-water mist nozzle to perform high-pressure spray molding, and drying the spray-formed microcapsules to obtain the antibacterial microcapsule modifier.

6. A fabric antibacterial function modifier and a preparation method thereof according to claim 5, characterized in that: The homogenization conditions are room temperature and pressure of 35-45MPa.

7. A fabric antibacterial function modifier and a preparation method thereof according to claim 5, characterized in that: The spray drying conditions are an inlet air temperature of 180-200°C and an outlet air temperature of 80-100°C.

8. A fabric antibacterial function modifier and a preparation method thereof, characterized in that: Prepared by the preparation method according to any one of claims 1 to 7. The prepared microcapsules are introduced onto textiles by dipping, rolling baking, spraying and the like to obtain antibacterial fabrics.

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