Preparation method of phytic acid-nano silver-hydroxypropyl chitosan moisturizing antibacterial finishing agent

Abstract

The invention relates to the technical field of antibacterial finishing agents, and discloses a preparation method of a phytic acid-nano silver-hydroxypropyl chitosan moisturizing antibacterial finishing agent, and the preparation method comprises the following steps: S1, weighing raw materials according to the component proportion; s2, heating a phytic acid solution, adding a silver nitrate solution into the heated phytic acid solution, and then adding a PH value stabilizer to adjust the PH value to 5-8 to obtain a solution I; s3, adding a glucose solution into the solution I, and heating and stirring for reaction to obtain a solution II; s4, adding a surfactant and an antioxidant into the hydroxypropyl chitosan solution, and then performing homogenization treatment by using a homogenizer to obtain a solution III; s5, adding the solution III into a sodium tripolyphosphate solution, performing ultrasonic treatment, and mixing with a nano-silver solution to obtain a solution IV; and S6, heating the solution IV, adding the solution II in batches, adding a pH value stabilizer to adjust the pH value to 6-8, adding a flame retardant, and stirring and mixing to finally obtain a finished product of the moisturizing antibacterial finishing agent.

Description

Technical Field

[0001] The invention relates to the technical field of antibacterial finishing agents, and more specifically to a method for preparing a phytic acid-nanosilver-hydroxypropyl chitosan moisturizing antibacterial finishing agent. Background Art

[0002] Technological development and social progress have pushed people's living standards to a higher level. Ordinary textiles can no longer meet the needs of the market, and people's requirements for the comfort, functionality and safety of textiles are gradually increasing. Textiles with composite functions are very popular, such as new textiles with multiple functions such as moisturizing and antibacterial.

[0003] Chitosan is a natural molecular alkaline polysaccharide that can be decomposed into glucosamine under the action of lysozyme in the body and absorbed by the human body. Chitosan is abundant in source, non-toxic, and has good biocompatibility, so it has great application prospects in the pharmaceutical industry, beauty industry, and textile industry. However, chitosan has poor water solubility and is only soluble in weak acids, which limits its application. By introducing hydroxypropyl groups, changing the intermolecular structure, and weakening the intermolecular and intramolecular hydrogen bonds, its water solubility and reactivity are improved, and hydroxypropylated chitosan has good moisture absorption and moisture retention, antibacterial properties and other characteristics. However, its antibacterial property is weaker than that of inorganic antibacterial agents and cannot meet the market demand for high-efficiency antibacterial agents.

[0004] Large specific surface area, high surface activity, and strong adsorption capacity give nanosilver a broad-spectrum antibacterial activity. With high permeability, it can combine with the active groups in the protein molecules of bacteria and destroy the protein structure, so nanosilver has extremely strong bactericidal activity. The resistance of organic antimicrobial agents is increasing, and the research and application of non-resistant nanosilver in the antibacterial field have received widespread attention. With the large-scale application of nanosilver in textiles, researchers have found that the toxicity of nanosilver will be accumulated and become toxic to the liver, nerves, reproductive system, etc. of the human body. To reduce or eliminate the cumulative toxicity of nanosilver, the most fundamental thing is to regulate the release of nanosilver from the source. Therefore, researchers have developed a technology for fixing or coating nanosilver particles, which can also regulate the release of nanosilver without affecting the antibacterial effect of nanosilver.

[0005] Phytic acid is a natural organic compound containing phosphorus, which is commonly found in oilseeds, beans, nuts, and pollen. It plays an important role in many physiological activities, such as diabetes and prevention of vascular calcification. Phytic acid also has a strong ability to chelate metals, and can form anionic micelles in aqueous solution to complex metal cations, such as silver, calcium, magnesium, zinc and other metal ions.

[0006] Therefore, combining the respective advantages of natural moisturizing and antibacterial chitosan and broad-spectrum antibacterial nano-silver to efficiently obtain a composite functional textile finishing agent with excellent moisturizing, broad-spectrum antibacterial, and reduced cumulative toxicity, while achieving the composite functions and reducing the use of toxic solvents and environmental pollution, is still a technical hurdle that needs to be overcome in this field. Summary of the invention

[0007] In order to overcome the shortcomings of the prior art, the present invention provides a method for preparing a phytic acid-nanosilver-hydroxypropyl chitosan moisturizing and antibacterial finishing agent, which has the advantage of more precise operation.

[0008] To achieve the above purpose, the present invention provides the following technical scheme: a phytic acid-nanosilver-hydroxypropyl chitosan moisturizing and antibacterial finishing agent, which is composed of the following raw materials in weight percentage: 10-70 parts of phytic acid solution, 5-15 parts of nanosilver solution, 5-15 parts of silver nitrate solution, 5-15 parts of glucose solution, 6-10 parts of hydroxypropyl chitosan solution, 6-10 parts of sodium tripolyphosphate solution, 0.8-3.5 parts of pH stabilizer, 0.1-0.6 parts of surfactant, 0.1-0.6 parts of antioxidant, and 0.1-0.6 parts of flame retardant surfactant.

[0009] As a preferred technical solution of the present invention, the present invention also provides a method for preparing a phytic acid-nanosilver-hydroxypropyl chitosan moisturizing and antibacterial finishing agent, comprising the following steps:

[0010] S1. Weigh each raw material according to the proportion of ingredients;

[0011] S2, heating the phytic acid solution, adding a silver nitrate solution to the heated phytic acid solution, and then adding a pH stabilizer to adjust the pH value to 5-8 to obtain a solution 1;

[0012] S3, adding glucose solution to solution 1, heating and stirring to react, to obtain solution 2;

[0013] S4, adding a surfactant and an antioxidant to the hydroxypropyl chitosan solution, and then homogenizing it using a homogenizer to obtain a solution three;

[0014] S5, adding solution 3 to the sodium tripolyphosphate solution, performing ultrasonic treatment, and mixing with the nanosilver solution to obtain solution 4;

[0015] S6. After heating solution 4, solution 2 is added in batches, a pH stabilizer is added to adjust the pH value to 6-8, and then a flame retardant is added and stirred to finally obtain a finished moisturizing and antibacterial finishing agent.

[0016] As a preferred technical solution of the present invention, in step S2, the phytic acid solution is heated to 35°C to 45°C and then the phytic acid solution is added; then the mixture is stirred using a stirring device, the stirring time is 30min to 60min, the stirring speed is 60r / min to 80r / min, and a pH stabilizer is added during the stirring process.

[0017] As a preferred technical solution of the present invention, in step S3, glucose solution is added and heated to 80°C to 95°C, and then the mixture is stirred using a stirring device for 20min to 40min at a stirring speed of 40r / min to 60r / min.

[0018] As a preferred technical solution of the present invention, in step S4, the hydroxypropyl chitosan solution, surfactant and antioxidant are stirred before homogenization, the stirring time is 20min to 40min, and the stirring speed is 40r / min to 60r / min; the speed of the homogenizer is 15000r / min to 20000r / min, and the processing time is 5min to 25min.

[0019] As a preferred technical solution of the present invention, in step S5, the solution is heated to a temperature of 60°C to 80°C before ultrasonic treatment, and then ultrasonic treatment is performed for 20min to 30min.

[0020] As a preferred technical solution of the present invention, in step S6, the solution is heated in a water bath at a temperature of 85°C to 95°C; after adding the flame retardant, the mixture is fully stirred and mixed for 40min to 80min at a stirring speed of 80r / min to 120r / min.

[0021] As a preferred technical solution of the present invention, in step S6, solution 2 is added to solution 4 being heated in three batches, and the ratio of the three batches of solution 2 is 1:2-4:3-6.

[0022] As a preferred technical solution of the present invention, the present invention also provides a use of a phytic acid-nanosilver-hydroxypropyl chitosan moisturizing and antibacterial finishing agent, wherein the above-mentioned phytic acid-nanosilver-hydroxypropyl chitosan moisturizing and antibacterial finishing agent is applied to pure cellulose fabrics or blended fabrics containing cellulose to prepare antibacterial fabrics.

[0023] Compared with the prior art, the invention has the following beneficial effects: the invention obtains the antibacterial and bactericidal ability of silver ions by adding nano silver and silver nitrate into the antibacterial finishing agent, and uses phytic acid as the main raw material. Phytic acid is a natural organic phosphoric acid compound with a phosphorus content of up to 28.16%. As a renewable, pure natural and pollution-free biological material, cellulose fibers will not produce substances that are toxic to the human body and the environment during the finishing process; the prepared antibacterial finishing agent can impart moisturizing and antibacterial functions to various textiles including towels, handkerchiefs, bedding, underwear, outerwear, socks, shoe fabrics, decorative fabrics, air filter materials, etc. DETAILED DESCRIPTION

[0024] The following will be combined with the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative work are within the scope of protection of the present invention.

[0025] Embodiment 1:

[0026] A method for preparing a phytic acid-nanosilver-hydroxypropyl chitosan moisturizing and antibacterial finishing agent comprises the following steps:

[0027] S1. Weigh the raw materials according to the following proportions:

[0028] 42 parts of phytic acid solution, 11 parts of nanosilver solution, 12 parts of silver nitrate solution, 8 parts of glucose solution, 8 parts of hydroxypropyl chitosan solution, 7 parts of sodium tripolyphosphate solution, 2.2 parts of pH stabilizer, 0.4 parts of surfactant, 0.4 parts of antioxidant, 0.3 parts of flame retardant surfactant;

[0029] S2, the phytic acid solution is heated to 40°C and then the phytic acid solution is added, and then the mixture is stirred by a stirring device for 45 minutes at a stirring speed of 70 r / min, and a pH stabilizer is added during the stirring process to adjust the pH value to 6.5 to obtain solution 1;

[0030] S3, adding glucose solution to solution 1, heating the glucose solution to 87°C, and then stirring the mixture with a stirring device for 30 minutes at a stirring speed of 50 r / min to obtain solution 2;

[0031] S4, adding a surfactant and an antioxidant to the hydroxypropyl chitosan solution, stirring the hydroxypropyl chitosan solution, the surfactant and the antioxidant for 30 min at a stirring speed of 50 r / min; then using a homogenizer for homogenization at a speed of 17500 r / min for 15 min to obtain solution three;

[0032] S5, after adding solution three to the sodium tripolyphosphate solution, heating the solution to a temperature of 70° C.; then using ultrasonic treatment for 25 min, mixing with the nanosilver solution to obtain solution four;

[0033] S6. Heat solution 4 in a water bath at a temperature of 90°C; then add solution 2 in three batches, and the ratio of the three batches of solution 2 is 1:3:5; then add a pH stabilizer to adjust the pH value to 7.2, add a flame retardant and stir well to mix, the stirring time is 60 minutes, the stirring speed is 100 r / min, and finally a finished moisturizing and antibacterial finishing agent is obtained.

[0034] The invention discloses a use of a phytic acid-nanosilver-hydroxypropyl chitosan moisturizing and antibacterial finishing agent. The phytic acid-nanosilver-hydroxypropyl chitosan moisturizing and antibacterial finishing agent prepared by the above method is applied to pure cellulose fabrics or blended fabrics containing cellulose to prepare antibacterial fabrics.

[0035] Embodiment 2:

[0036] A method for preparing a phytic acid-nanosilver-hydroxypropyl chitosan moisturizing and antibacterial finishing agent comprises the following steps:

[0037] S1. Weigh the raw materials according to the following proportions:

[0038] 23 parts of phytic acid solution, 5 parts of nanosilver solution, 6 parts of silver nitrate solution, 6 parts of glucose solution, 7 parts of hydroxypropyl chitosan solution, 6 parts of sodium tripolyphosphate solution, 0.8 parts of pH stabilizer, 0.2 parts of surfactant, 0.1 parts of antioxidant, 0.2 parts of flame retardant surfactant;

[0039] S2, heating the phytic acid solution to 35°C and then adding the phytic acid solution, and then stirring the mixture with a stirring device for 30 minutes at a stirring speed of 60r / min, and adding a pH stabilizer during the stirring process to adjust the pH value to 5.2 to obtain solution 1;

[0040] S3, adding glucose solution to solution 1, heating the glucose solution to 80°C, and then stirring the mixture with a stirring device for 20 minutes at a stirring speed of 40 r / min to obtain solution 2;

[0041] S4, adding a surfactant and an antioxidant to the hydroxypropyl chitosan solution, stirring the hydroxypropyl chitosan solution, the surfactant and the antioxidant for 20 min at a stirring speed of 40 r / min; then using a homogenizer for homogenization at a speed of 15000 r / min for 5 min to obtain solution three;

[0042] S5, after adding solution three to the sodium tripolyphosphate solution, heating the solution to a temperature of 60° C.; then using ultrasonic treatment for 20 minutes, mixing with the nanosilver solution to obtain solution four;

[0043] S6. Heat solution 4 in a water bath at a temperature of 85°C; then add solution 2 in three batches, and the ratio of the three batches of solution 2 is 1:2:3; then add a pH stabilizer to adjust the pH value to 6.2, add the flame retardant and stir well to mix, the stirring time is 40 minutes, the stirring speed is 80r / min, and finally obtain a finished moisturizing and antibacterial finishing agent.

[0044] The invention discloses a use of a phytic acid-nanosilver-hydroxypropyl chitosan moisturizing and antibacterial finishing agent. The phytic acid-nanosilver-hydroxypropyl chitosan moisturizing and antibacterial finishing agent prepared by the above method is applied to pure cellulose fabrics or blended fabrics containing cellulose to prepare antibacterial fabrics.

[0045] Embodiment three:

[0046] A method for preparing a phytic acid-nanosilver-hydroxypropyl chitosan moisturizing and antibacterial finishing agent comprises the following steps:

[0047] S1. Weigh the raw materials according to the following proportions:

[0048] 66 parts of phytic acid solution, 14 parts of nanosilver solution, 12 parts of silver nitrate solution, 13 parts of glucose solution, 9 parts of hydroxypropyl chitosan solution, 9 parts of sodium tripolyphosphate solution, 3.2 parts of pH stabilizer, 0.5 parts of surfactant, 0.5 parts of antioxidant, 0.5 parts of flame retardant surfactant;

[0049] S2, the phytic acid solution is heated to 45°C and then the phytic acid solution is added, and then the mixture is stirred by a stirring device for 60 minutes at a stirring speed of 80 r / min, and a pH stabilizer is added during the stirring process to adjust the pH value to 7.2 to obtain solution 1;

[0050] S3, adding glucose solution to solution one, heating the glucose solution to 95°C, and then stirring the mixture with a stirring device for 40 minutes at a stirring speed of 60 r / min to obtain solution two;

[0051] S4, adding a surfactant and an antioxidant to the hydroxypropyl chitosan solution, stirring the hydroxypropyl chitosan solution, the surfactant and the antioxidant for 40 min at a stirring speed of 60 r / min; then using a homogenizer for homogenization at a speed of 20000 r / min for 25 min to obtain solution three;

[0052] S5, after adding solution three to the sodium tripolyphosphate solution, heating the solution to 80° C.; then using ultrasonic treatment for 30 min, mixing with the nanosilver solution to obtain solution four;

[0053] S6. Heat solution 4 in a water bath at a temperature of 95°C; then add solution 2 in three batches, and the ratio of the three batches of solution 2 is 1:4:5; then add a pH stabilizer to adjust the pH value to 7.4, add a flame retardant and stir well to mix, the stirring time is 80 minutes, the stirring speed is 120r / min, and finally obtain a finished moisturizing and antibacterial finishing agent.

[0054] The invention discloses a use of a phytic acid-nanosilver-hydroxypropyl chitosan moisturizing and antibacterial finishing agent. The phytic acid-nanosilver-hydroxypropyl chitosan moisturizing and antibacterial finishing agent prepared by the above method is applied to pure cellulose fabrics or blended fabrics containing cellulose to prepare antibacterial fabrics.

[0055] The finishing agents prepared in Example 1, Example 2, Example 3 and the existing finishing agent group and the reference group were used to immerse the fabrics, and then the antibacterial test was carried out. The fabric materials used in the examples and the comparative examples are exactly the same.

[0056] The impregnation treatment process is to immerse the textile material in the corresponding antibacterial finishing agent at room temperature for 180 seconds, and then dry it at 90°C after the treatment; the dried textile material is heat-treated at 160°C for 20 seconds to obtain the antibacterial finished textile material.

[0057] The antibacterial test was carried out according to the national standard GB / T20944.2-2007 “Evaluation of Antibacterial Properties of Textiles Part 2: Absorption Method”, using Escherichia coli and Staphylococcus aureus for antibacterial performance testing.

[0058] The fabrics corresponding to the Example 1, Example 2, Example 3 and the reference group were washed 50 times under the same conditions, and the antibacterial properties before and after washing are as follows:

[0059] Embodiment 1 Embodiment 2 Embodiment 3 Reference group Escherichia coli inhibition rate (%) 96.4 97.4 97.6 73.1 Staphylococcus aureus inhibition rate (%) 98.4 97.9 98.1 74.6

[0060] It can be intuitively obtained from the above table that the fabric treated with the finishing agent prepared by the present invention has better antibacterial and antimicrobial properties than the traditional finishing agent.

[0061] It should be noted that, in this article, relational terms such as first and second, etc. are only used to distinguish one entity or operation from another entity or operation, and do not necessarily require or imply any such actual relationship or order between these entities or operations. Moreover, the terms "include", "comprise" or any other variants thereof are intended to cover non-exclusive inclusion, so that a process, method, article or device including a series of elements includes not only those elements, but also other elements not explicitly listed, or also includes elements inherent to such process, method, article or device.

[0062] Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and variations may be made to the embodiments without departing from the principles and spirit of the present invention, and that the scope of the present invention is defined by the appended claims and their equivalents.

Claims

1. A phytic acid-nanosilver-hydroxypropyl chitosan moisturizing and antibacterial finishing agent, characterized in that: The invention is composed of the following raw materials in percentage by weight: 10-70 parts of phytic acid solution, 5-15 parts of nano silver solution, 5-15 parts of silver nitrate solution, 5-15 parts of glucose solution, 6-10 parts of hydroxypropyl chitosan solution, 6-10 parts of sodium tripolyphosphate solution, 0.8-3.5 parts of pH value stabilizer, 0.1-0.6 parts of surfactant, 0.1-0.6 parts of antioxidant and 0.1-0.6 parts of flame retardant surfactant.

2. The method for preparing a phytic acid-nanosilver-hydroxypropyl chitosan moisturizing and antibacterial finishing agent according to claim 1, characterized in that: The steps include: S1. Weigh each raw material according to the proportion of ingredients; S2, heating the phytic acid solution, adding a silver nitrate solution to the heated phytic acid solution, and then adding a pH stabilizer to adjust the pH value to 5-8 to obtain a solution 1; S3, adding glucose solution to solution 1, heating and stirring to react, to obtain solution 2; S4, adding a surfactant and an antioxidant to the hydroxypropyl chitosan solution, and then homogenizing it using a homogenizer to obtain a solution three; S5, adding solution 3 to the sodium tripolyphosphate solution, performing ultrasonic treatment, and mixing with the nanosilver solution to obtain solution 4; S6. After heating solution 4, solution 2 is added in batches, a pH stabilizer is added to adjust the pH value to 6-8, and then a flame retardant is added and stirred to finally obtain a finished moisturizing and antibacterial finishing agent.

3. The method for preparing a phytic acid-nanosilver-hydroxypropyl chitosan moisturizing and antibacterial finishing agent according to claim 2, characterized in that: In the step S2, the phytic acid solution is heated to 35°C to 45°C and then the phytic acid solution is added; then the mixture is stirred using a stirring device, the stirring time is 30min to 60min, the stirring speed is 60r / min to 80r / min, and a pH stabilizer is added during the stirring process.

4. The method for preparing a phytic acid-nanosilver-hydroxypropyl chitosan moisturizing and antibacterial finishing agent according to claim 2, characterized in that: In the step S3, glucose solution is added and heated to 80°C to 95°C, and then the mixture is stirred by a stirring device for 20min to 40min at a stirring speed of 40r / min to 60r / min.

5. The method for preparing a phytic acid-nanosilver-hydroxypropyl chitosan moisturizing and antibacterial finishing agent according to claim 2, characterized in that: In the step S4, the hydroxypropyl chitosan solution, surfactant and antioxidant are stirred before homogenization, the stirring time is 20min to 40min, and the stirring speed is 40r / min to 60r / min; the speed of the homogenizer is 15000r / min to 20000r / min, and the processing time is 5min to 25min.

6. The method for preparing a phytic acid-nanosilver-hydroxypropyl chitosan moisturizing and antibacterial finishing agent according to claim 2, characterized in that: In the step S5, the solution is heated to a temperature of 60°C to 80°C before the ultrasonic treatment, and then ultrasonic treatment is performed for 20 minutes to 30 minutes.

7. The method for preparing a phytic acid-nanosilver-hydroxypropyl chitosan moisturizing and antibacterial finishing agent according to claim 2, characterized in that: In the step S6, the solution is heated in a water bath at a temperature of 85° C. to 95° C. After the flame retardant is added, the mixture is stirred and mixed thoroughly for a stirring time of 40 min to 80 min and a stirring speed of 80 r / min to 120 r / min.

8. The method for preparing a phytic acid-nanosilver-hydroxypropyl chitosan moisturizing and antibacterial finishing agent according to claim 2, characterized in that: In step S6, solution 2 is added to the heated solution 4 in three batches, and the ratio of the three batches of solution 2 is 1:2-4:3-6.

9. Use of a phytic acid-nanosilver-hydroxypropyl chitosan moisturizing and antibacterial finishing agent, characterized in that: The phytic acid-nanosilver-hydroxypropyl chitosan moisturizing and antibacterial finishing agent described in claim 1 is applied to pure cellulose fabrics or blended fabrics containing cellulose to prepare antibacterial fabrics.