Preparation Method and Application of a Zinc Oxide Antibacterial Finishing Agent

By preparing zinc oxide suspension and adding appropriate additives to prepare zinc oxide antibacterial finishing agent, the dispersion and washing resistance of nano zinc oxide powder in textiles are solved, and efficient and long-lasting antibacterial effect is achieved.

CN116084157BActive Publication Date: 2025-07-22JINDA NAMI TECH XIAMEN CO LTD
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Patent Information

Application Number
CN202310271222.6
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2023-03-20
Publication Date
2025-07-22
Estimated Expiration
2043-03-20

AI Technical Summary

Technical Problem

In the prior art, nano zinc oxide powders have problems such as difficult to disperse, easy to agglomerate, not resistant to water washing, and not lasting antibacterial effects in textile finishing agents.

Method used

By preparing zinc oxide suspension, adding wetting agent, dispersion stabilizer, pH adjuster and defoaming agent, dispersion agent, and defoaming agent, it is configured as zinc oxide suspension, and then adding binder, penetrant and crosslinking agent to prepare zinc oxide antibacterial finishing agent to ensure that the zinc oxide particle size is small and the distribution is narrow, and high dispersion is achieved.

Benefits of technology

The prepared zinc oxide antibacterial finishing agent has a good bonding fastness to textile fabrics, and can still maintain good antibacterial performance after several washings, achieving efficient and long-lasting antibacterial effects.

✦ Generated by Eureka AI based on patent content.

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Abstract

The present invention relates to a preparation method and application of a zinc oxide antibacterial finishing agent, comprising the following steps: S1. Prepare a zinc oxide suspension: Add zinc oxide powder and a wetting agent to a part of water, stir for 0.5 - 1 h, then add a dispersion stabilizer and stir for 0.5 - 1 h. After that, add a pH regulator and stir thoroughly, then add the remaining water and stir thoroughly. Further, grind and disperse at a first stirring rate for 2 h, then grind and disperse at a second stirring rate for 13 - 14 h. Finally, add an antifoaming agent and grind and disperse at a third stirring rate for 0.5 h to obtain the zinc oxide suspension; S2. Prepare the zinc oxide antibacterial finishing agent: Stir the prepared zinc oxide suspension, binder, penetrant and crosslinking agent thoroughly at the third stirring rate. The zinc oxide prepared by the present invention can maintain high dispersibility during application, and can endow the fabric with excellent antibacterial properties without the cooperation of other antibacterial agents. Moreover, the finishing agent prepared by this method has good bonding fastness with a variety of textile fabrics and can still maintain good antibacterial properties after being washed several times.
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Description

Technical Field

[0001] The present invention relates to the technical field of textiles, and particularly to a preparation method and application of a zinc oxide antibacterial finishing agent. Background Art

[0002] As is well known, there are various bacteria in the environment where humans live. With the improvement of people's living standards, the demand for healthy and environmentally friendly fabrics is also increasing day by day. Due to the porous and loose structure of textiles, it is extremely easy to cause the growth and reproduction of microorganisms. Endowing fabrics with antibacterial functions through textile fabric post-treatment processes is the simplest and lowest-cost method. Therefore, the development and research of efficient textile antibacterial finishing agents have emerged as the times require.

[0003] There are many types of antibacterial finishing agents applied to textiles, mainly including organic, inorganic, natural antibacterial agents, and polymer antibacterial agents. Nano-zinc oxide is a common inorganic antibacterial agent. Due to its high safety, excellent antibacterial properties, and good heat resistance, it has become a rising star among antibacterial agents. However, when used alone, nano-powders have problems such as difficult dispersion, easy agglomeration, and poor wash-fastness performance, which also restricts its application to a certain extent. Therefore, it is urgent to develop a zinc oxide antibacterial finishing agent that can be stored for a long time under conventional conditions and has good binding force with fabrics and excellent antibacterial performance in the post-treatment of textiles.

[0004] Chinese Patent CN105019236A discloses a textile composite antibacterial finishing agent. The prepared product has high heat resistance, strong antibacterial properties, is safe and reliable, and is green and environmentally friendly. However, other antibacterial agents still need to be synergistically combined with nano-zinc oxide to achieve better antibacterial effects. Summary of the Invention

[0005] The technical problem to be solved by the present invention is: The present invention provides a preparation method and application of a zinc oxide antibacterial finishing agent to solve the problems of difficult dispersion, easy agglomeration, poor wash-fastness, and non-persistent antibacterial effect when directly applying zinc oxide powder to the finishing agent in the prior art.

[0006] To solve the above technical problems, the technical solution adopted by the present invention is:

[0007] The first aspect of the present invention provides a preparation method of a zinc oxide antibacterial finishing agent, including the following steps:

[0008] S1. Prepare a zinc oxide suspension: Add zinc oxide powder and a wetting agent to a part of water, stir for 0.5 - 1 h, then add a dispersion stabilizer and stir for 0.5 - 1 h. Then add a pH regulator and stir thoroughly, and then add the remaining water and stir thoroughly. Further, grind and disperse at a first stirring rate for 2 h, then grind and disperse at a second stirring rate for 13 - 14 h, and finally add an antifoaming agent and grind and disperse at a third stirring rate for 0.5 h to obtain the zinc oxide suspension;

[0009] S2. Prepare the zinc oxide antibacterial finishing agent: Stir the prepared zinc oxide suspension, binder, penetrant and crosslinking agent at the third stirring rate sufficiently.

[0010] A preparation method of a zinc oxide antibacterial finishing agent proposed by the present invention uses zinc oxide powder as the main functional raw material, supplemented with a wetting agent, a dispersion stabilizer, a pH regulator and an antifoaming agent to prepare a zinc oxide suspension. The D50 of the zinc oxide particle size in the finally obtained zinc oxide suspension is 0.4 - 0.5 μm, with small particle size and narrow particle size distribution. Then, a binder, a penetrant and a crosslinking agent are added to prepare the finishing agent. The zinc oxide prepared by this process can maintain high dispersibility during application, and can endow the fabric with excellent antibacterial properties without the cooperation of other antibacterial agents. Moreover, the finishing agent prepared by this method has good bonding fastness with various textile fabrics and can still maintain good antibacterial properties after being washed several times.

[0011] Optionally, in step S1: The particle size of the zinc oxide powder is 1 - 50 μm.

[0012] Optionally, in step S1: The zinc oxide powder accounts for 10 - 35% of the total mass of the suspension; the wetting agent accounts for 0.1 - 1% of the mass of the zinc oxide powder; the dispersion stabilizer accounts for 1 - 15% of the mass of the zinc oxide powder; the pH regulator accounts for 0.1 - 3% of the total mass of the suspension, and it is diluted by 10 - 30% in advance before adding; the antifoaming agent accounts for 0.01 - 0.1% of the total mass of the suspension; the rest is water.

[0013] Optionally, in step S1: The wetting agent is a fatty alcohol polyoxyethylene ether; the dispersion stabilizer is one or more of sodium polyacrylate, polyacrylate, sodium polycarboxylate, ammonium polycarboxylate, dodecylbenzenesulfonate; the pH regulator is one or more of citric acid, oxalic acid, sodium citrate, potassium citrate, sodium hydroxide; the antifoaming agent is one or more of fatty acids, fatty acid esters, phosphate esters, polyether-modified silicone.

[0014] Optionally, in step S2: By mass percentage: 80 - 98% of zinc oxide suspension, 0.5 - 15% of binder, 0.5 - 5% of penetrant, 0.5 - 5% of crosslinking agent.

[0015] Optionally, in step S2: the adhesive is one or more of acrylic resin, polyvinyl alcohol resin, water-based polyurethane resin, and carboxymethyl cellulose; the penetrant is one or more of sodium secondary alkyl sulfonate, sodium α-olefin sulfonate, sodium alkyl naphthalene sulfonate, sodium alkyl succinate sulfonate, sodium aminosulfonate, and fatty alcohol polyoxyethylene ether; the cross-linking agent is one or more of a polyfunctional aziridine cross-linking agent, an isocyanate cross-linking agent, a polyaziridine cross-linking agent, and an aziridine-modified isocyanate cross-linking agent.

[0016] Optionally, the first stirring rate is 300-400 r / min, the second stirring rate is 600-800 r / min, and the third stirring rate is 100-200 r / min.

[0017] The second aspect of the present invention provides an application of a zinc oxide antibacterial finishing agent in a textile product. When applied to the post-finishing of textile fabrics, the zinc oxide antibacterial finishing agent is added at a ratio of 4-10%, the water bath ratio is 1:10-1:20, and then the fabric is impregnated, pre-baked, and baked to obtain a fabric containing the zinc oxide antibacterial finishing agent.

[0018] According to the above description, the zinc oxide antibacterial finishing agent can be widely used in finishing various textile fabrics to prepare antibacterial fabrics, and the prepared antibacterial fabrics have high-efficiency and long-lasting antibacterial properties. DETAILED DESCRIPTION

[0019] The technical solutions in the embodiments of the present invention are described clearly and completely below. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of them. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0020] The embodiment of the present invention provides a method for preparing a zinc oxide antibacterial finishing agent, comprising the following steps:

[0021] S1. Prepare a zinc oxide suspension: add zinc oxide powder and a wetting agent to part of the water, stir for 0.5-1h, then add a dispersion stabilizer and stir for 0.5-1h, then add a pH adjuster and stir sufficiently, then add the remaining water and stir sufficiently, further grind and disperse at a first stirring rate for 2h, then grind and disperse at a second stirring rate for 13-14h, finally add a defoamer, and grind and disperse at a third stirring rate for 0.5h to obtain a zinc oxide suspension;

[0022] S2. Preparing a zinc oxide antibacterial finishing agent: fully stirring the prepared zinc oxide suspension, adhesive, penetrant and cross-linking agent at a third stirring rate.

[0023] Preferably, the sufficient stirring time is 30-40 minutes.

[0024] In step S1: the particle size of the zinc oxide powder is 1 - 50 μm.

[0025] Preferably, the particle size of the zinc oxide powder is 2 - 10 μm.

[0026] In step S1: the zinc oxide powder is 10 - 35% of the total mass of the suspension; the wetting agent is 0.1 - 1% of the mass of the zinc oxide powder; the dispersion stabilizer is 1 - 15% of the mass of the zinc oxide powder; the pH regulator is 0.1 - 3% of the total mass of the suspension, and it is diluted by 10 - 30% in advance before addition; the defoaming agent is 0.01 - 0.1% of the total mass of the suspension; the rest is water.

[0027] Preferably, the zinc oxide powder is 15 - 30% of the total mass of the suspension; the wetting agent is 0.4 - 0.8% of the mass of the zinc oxide powder; the dispersion stabilizer is 5 - 10% of the mass of the zinc oxide powder; the pH regulator is 0.2 - 2% of the total mass of the suspension; the defoaming agent is 0.01 - 0.03% of the total mass of the suspension; the rest is water.

[0028] In step S1: the wetting agent is fatty alcohol polyoxyethylene ether; the dispersion stabilizer is one or more of sodium polyacrylate, polyacrylate, sodium polycarboxylate, ammonium polycarboxylate, dodecylbenzenesulfonate; the pH regulator is one or more of citric acid, oxalic acid, sodium citrate, potassium citrate, sodium hydroxide; the defoaming agent is one or more of fatty acids, fatty acid esters, phosphate esters, polyether modified silicone.

[0029] Preferably, the dispersion stabilizer is one or more of polyacrylic acid, ammonium polyacrylate, sodium polyacrylate, dodecylbenzenesulfonate.

[0030] In step S2: by mass percentage: 80 - 98% of zinc oxide suspension, 0.5 - 15% of binder, 0.5 - 5% of penetrant, 0.5 - 5% of crosslinking agent.

[0031] Preferably, the zinc oxide suspension is 90 - 95% of the total mass of the finishing agent; the binder is 2 - 10% of the total mass of the finishing agent; the penetrant is 0.5 - 2% of the total mass of the finishing agent; the crosslinking agent is 0.5 - 2.5% of the total mass of the finishing agent.

[0032] In step S2: The binder is one or more of acrylic resin, polyvinyl alcohol resin, waterborne polyurethane resin, and carboxymethyl cellulose; the penetrant is one or more of secondary alkyl sulfonate, α-olefin sulfonate, alkyl naphthalene sulfonate, alkyl succinate sulfonate, sodium aminosulfonate, and fatty alcohol polyoxyethylene ether; the crosslinking agent is one or more of multifunctional aziridine crosslinking agent, isocyanate crosslinking agent, polyaziridine crosslinking agent, and aziridine-modified isocyanate crosslinking agent.

[0033] The first stirring rate is 300 - 400 r / min, the second stirring rate is 600 - 800 r / min, and the third stirring rate is 100 - 200 r / min.

[0034] When applying the above zinc oxide antibacterial finishing agent to the post-finishing of textile fabrics, add the zinc oxide antibacterial finishing agent at a ratio of 4 - 10%, the bath ratio is 1:10 - 1:20, and then perform padding, pre-drying, and baking treatments to obtain a fabric containing the zinc oxide antibacterial finishing agent.

[0035] Preferably, the ratio is 4 - 6%.

[0036] Example 1

[0037] S1. Prepare a zinc oxide suspension:

[0038] Add 50 kg of zinc oxide powder and 0.25 kg of wetting agent to 100 kg of water, stir for 30 min, then add 5 kg of dispersion stabilizer and stir for 30 min. Then add 1.875 kg of pH regulator and stir thoroughly for 30 min. Add the remaining water and stir thoroughly for 30 min. Further grind and disperse at a rate of 400 r / min for 2 h, then grind and disperse at a rate of 700 r / min for 13 h. Finally, add 25 g of defoamer and grind and disperse at a rate of 100 r / min for 30 min to obtain a zinc oxide suspension with a D50 of 0.43 μm.

[0039] S2. Prepare a zinc oxide antibacterial finishing agent:

[0040] Mix the prepared zinc oxide suspension, binder, penetrant, and crosslinking agent in a mass ratio of 95%:3%:1%:1%, and stir at a rotation speed of 100 r / min for 30 min.

[0041] Among them, the D50 of the zinc oxide powder used in step S1 is 2 μm; the wetting agent used is fatty alcohol polyoxyethylene ether - 9; the dispersion stabilizer used is sodium polyacrylate; the pH regulator used is sodium citrate; the defoamer used is polyether-modified silicone; their mass ratio is zinc oxide powder: fatty alcohol polyoxyethylene ether - 9: sodium polyacrylate: sodium citrate: polyether-modified silicone = 20%:0.1%:2%:0.75%:0.01%.

[0042] In step S2, the adhesive used is acrylic resin; the penetrant used is fatty alcohol polyoxyethylene ether; the crosslinking agent used is polyfunctional aziridine crosslinking agent.

[0043] Example 2

[0044] S1. Prepare zinc oxide suspension:

[0045] Add 75 kg of zinc oxide powder and 0.25 kg of wetting agent to 100 kg of water, stir for 30 min, then add 7.5 kg of dispersion stabilizer and stir for 30 min. After that, add 0.5 kg of pH regulator and stir thoroughly for 30 min. Then add the remaining water and stir thoroughly for 30 min. Further grind and disperse at a rate of 400 r / min for 2 h, then grind and disperse at a rate of 800 r / min for 14 h. Finally, add 25 g of defoamer and grind and disperse at a rate of 100 r / min for 30 min to obtain a zinc oxide suspension with a D50 of 0.49 μm.

[0046] S2. Prepare zinc oxide antibacterial finishing agent:

[0047] Mix the prepared zinc oxide suspension, adhesive, penetrant and crosslinking agent according to a mass ratio of 92%:5%:1%:2%, and stir at a rotation speed of 100 r / min for 30 min.

[0048] Among them, the D50 of the zinc oxide powder used in step S1 is 3 μm; the wetting agent used is fatty alcohol polyoxyethylene ether-9; the dispersion stabilizer used is ammonium polyacrylate; the pH regulator used is citric acid; the defoamer used is polyether-modified silicone; and their mass ratio is zinc oxide powder: fatty alcohol polyoxyethylene ether-9: ammonium polyacrylate: citric acid: polyether-modified silicone = 30%:0.1%:3%:0.2%:0.01%.

[0049] In step S2, the adhesive used is acrylic resin; the penetrant used is fatty alcohol polyoxyethylene ether; the crosslinking agent used is polyfunctional aziridine crosslinking agent.

[0050] Example 3

[0051] S1. Prepare zinc oxide suspension:

[0052] Add 50 kg of zinc oxide powder and 0.25 kg of wetting agent to 100 kg of water, stir for 30 min, then add 7.5 kg of dispersion stabilizer and stir for 30 min. Then add 0.5 kg of pH regulator and stir thoroughly for 30 min. Then add the remaining water and stir thoroughly for 30 min. Further grind and disperse at a rate of 300 r / min for 2 h, then grind and disperse at a rate of 800 r / min for 13 h. Finally, add 50 g of defoamer and grind and disperse at a rate of 100 r / min for 30 min to obtain a zinc oxide suspension with a D50 of 0.45 μm;

[0053] S2. Prepare zinc oxide antibacterial finishing agent:

[0054] Mix the prepared zinc oxide suspension, binder, penetrant and crosslinking agent according to a mass ratio of 93%:5%:1%:1%, and stir at a rotation speed of 100 r / min for 30 min.

[0055] Among them, the zinc oxide powder used in step S1 has a D50 of 2.5 μm; the wetting agent used is fatty alcohol polyoxyethylene ether-10; the dispersion stabilizer used is sodium polyacrylate and polyacrylic acid; the pH regulator used is sodium hydroxide; the defoamer used is polyether-modified silicone; and their mass ratio is zinc oxide powder: fatty alcohol polyoxyethylene ether-10: sodium polyacrylate: polyacrylic acid: sodium hydroxide: polyether-modified silicone = 20%:0.1%:1.5%:1.5%:0.2%:0.02%.

[0056] The binder used in step S2 is polyvinyl alcohol; the penetrant used is fatty alcohol polyoxyethylene ether; the crosslinking agent used is multifunctional aziridine crosslinking agent.

[0057] Example 4

[0058] S1. Prepare zinc oxide suspension:

[0059] Add 50 kg of zinc oxide powder and 0.25 kg of wetting agent to 100 kg of water, stir for 30 min, then add 2.5 kg of dispersion stabilizer and stir for 30 min. Then add 0.75 kg of pH regulator and stir thoroughly for 30 min. Then add the remaining water and stir thoroughly for 30 min. Further grind and disperse at a rate of 300 r / min for 2 h, then grind and disperse at a rate of 700 r / min for 13 h. Finally, add 50 g of defoamer and grind and disperse at a rate of 100 r / min for 30 min to obtain a zinc oxide suspension with a D50 of 0.47 μm;

[0060] S2. Prepare zinc oxide antibacterial finishing agent:

[0061] Mix the prepared zinc oxide suspension, binder, penetrant, and crosslinking agent in a mass ratio of 95%:3%:1%:1%, and stir for 30 minutes at a rotation speed of 100 r / min.

[0062] Among them, the D50 of the zinc oxide powder used in step S1 is 2 μm; the wetting agent used is fatty alcohol polyoxyethylene ether-9; the dispersion stabilizer used is sodium dodecylbenzenesulfonate; the pH regulator used is sodium citrate; the defoaming agent used is polyether-modified silicone; and their mass ratio is zinc oxide powder: fatty alcohol polyoxyethylene ether-9: sodium dodecylbenzenesulfonate: sodium citrate: polyether-modified silicone = 20%:0.1%:1%:0.3%:0.02%.

[0063] The binder used in step S2 is polyvinyl alcohol; the penetrant used is fatty alcohol polyoxyethylene ether; the crosslinking agent used is polyfunctional aziridine crosslinking agent.

[0064] Example 5

[0065] S1. Prepare zinc oxide suspension:

[0066] Add 75 kg of zinc oxide powder and 0.25 kg of wetting agent to 100 kg of water, stir for 30 minutes, then add 7.5 kg of dispersion stabilizer and stir for 30 minutes. Then add 0.5 kg of pH regulator and stir thoroughly for 30 minutes. Add the remaining water and stir thoroughly for 30 minutes. Further grind and disperse at a rate of 400 r / min for 2 hours, then grind and disperse at a rate of 800 r / min for 14 hours. Finally, add 50 g of defoaming agent and grind and disperse at a rate of 100 r / min for 30 minutes to obtain a zinc oxide suspension with D50 of 0.42 μm.

[0067] S2. Prepare zinc oxide antibacterial finishing agent:

[0068] Mix the prepared zinc oxide suspension, binder, penetrant, and crosslinking agent in a mass ratio of 94%:3%:1.5%:1.5%, and stir for 30 minutes at a rotation speed of 100 r / min.

[0069] Among them, the D50 of the zinc oxide powder used in step S1 is 2 μm; the wetting agent used is fatty alcohol polyoxyethylene ether-9; the dispersion stabilizer used is sodium polyacrylate; the pH regulator used is citric acid; the defoaming agent used is fatty acid ester; and their mass ratio is zinc oxide powder: fatty alcohol polyoxyethylene ether-9: sodium polyacrylate: citric acid: fatty acid ester = 30%:0.1%:3%:0.2%:0.02%.

[0070] The binder used in step S2 is acrylic resin; the penetrant used is secondary alkyl sulfonate; the crosslinking agent used is polyfunctional aziridine crosslinking agent.

[0071] Example 6

[0072] S1. Prepare zinc oxide suspension:

[0073] Add 50 kg of zinc oxide powder and 0.25 kg of wetting agent to 100 kg of water, stir for 30 min, then add 7.5 kg of dispersion stabilizer and stir for 30 min. After that, add 2.5 kg of pH regulator and stir thoroughly for 30 min. Then add the remaining water and stir thoroughly for 30 min. Further grind and disperse at a rate of 300 r / min for 2 h, then grind and disperse at a rate of 700 r / min for 14 h. Finally, add 50 g of defoamer and grind and disperse at a rate of 100 r / min for 30 min to obtain a zinc oxide suspension with D50 of 0.43 μm;

[0074] S2. Prepare zinc oxide antibacterial finishing agent:

[0075] Mix the prepared zinc oxide suspension, binder, penetrant and crosslinking agent in a mass ratio of 92%:6%:1%:1%, and stir at a speed of 100 r / min for 30 min.

[0076] Among them, the D50 of the zinc oxide powder used in step S1 is 2 μm; the wetting agent used is fatty alcohol polyoxyethylene ether - 9; the dispersion stabilizer used is polyacrylic acid; the pH regulator used is sodium hydroxide; the defoamer used is polyether modified silicone; and their mass ratio is zinc oxide powder:fatty alcohol polyoxyethylene ether - 9:polyacrylic acid:sodium hydroxide:polyether modified silicone = 20%:0.1%:3%:1%:0.02%.

[0077] The binder used in step S2 is acrylic resin; the penetrant used is secondary alkyl sulfonate; the crosslinking agent used is polyfunctional aziridine crosslinking agent.

[0078] Example 7

[0079] S1. Prepare zinc oxide suspension:

[0080] Add 50 kg of zinc oxide powder and 0.25 kg of wetting agent to 100 kg of water, stir for 30 min, then add 7.5 kg of dispersion stabilizer and stir for 30 min. After that, add 0.5 kg of pH regulator and stir thoroughly for 30 min. Then add the remaining water and stir thoroughly for 30 min. Further grind and disperse at a rate of 350 r / min for 2 h, then grind and disperse at a rate of 750 r / min for 14 h. Finally, add 75 g of defoamer and grind and disperse at a rate of 100 r / min for 30 min to obtain a zinc oxide suspension with D50 of 0.44 μm;

[0081] S2. Prepare zinc oxide antibacterial finishing agent:

[0082] Mix the prepared zinc oxide suspension, binder, penetrant, and crosslinking agent in a mass ratio of 92%:6%:1%:1%, and stir for 30 minutes at a rotation speed of 100 r / min.

[0083] Among them, the D50 of the zinc oxide powder used in step S1 is 2 μm; the wetting agent used is fatty alcohol polyoxyethylene ether-9; the dispersion stabilizer used is polyacrylic acid and ammonium polyacrylate; the pH regulator used is sodium hydroxide; the defoaming agent used is fatty acid and polyether-modified silicone; their mass ratio is zinc oxide powder: fatty alcohol polyoxyethylene ether-9: polyacrylic acid: ammonium polyacrylate: sodium hydroxide: fatty acid: polyether-modified silicone = 20%:0.1%:1.5%:1.5%:0.2%:0.01%:0.02%.

[0084] The binder used in step S2 is polyvinyl alcohol; the penetrant used is secondary alkyl sulfonate; the crosslinking agent used is polyfunctional aziridine crosslinking agent.

[0085] Example 8

[0086] S1. Prepare zinc oxide suspension:

[0087] Add 50 kg of zinc oxide powder and 0.25 kg of wetting agent to 100 kg of water, stir for 30 minutes, then add 7.5 kg of dispersion stabilizer and stir for 30 minutes. Then add 0.5 kg of pH regulator and stir thoroughly for 30 minutes. Then add the remaining water and stir thoroughly for 30 minutes. Further grind and disperse at a rate of 350 r / min for 2 hours, and then grind and disperse at a rate of 750 r / min for 14 hours. Finally, add 50 g of defoaming agent and grind and disperse at a rate of 100 r / min for 30 minutes to obtain a zinc oxide suspension with D50 of 0.44 μm.

[0088] S2. Prepare zinc oxide antibacterial finishing agent:

[0089] Mix the prepared zinc oxide suspension, binder, penetrant, and crosslinking agent in a mass ratio of 93%:5%:1%:1%, and stir for 30 minutes at a rotation speed of 100 r / min.

[0090] Among them, the D50 of the zinc oxide powder used in step S1 is 2 μm; the wetting agent used is fatty alcohol polyoxyethylene ether-9; the dispersion stabilizer used is polyacrylic acid and ammonium polyacrylate; the pH regulator used is sodium hydroxide; the defoaming agent used is polyether-modified silicone and fatty acid; their mass ratio is zinc oxide powder: fatty alcohol polyoxyethylene ether-9: polyacrylic acid: ammonium polyacrylate: sodium hydroxide: polyether-modified silicone: fatty acid = 20%:0.1%:1.5%:1.5%:0.2%:0.01%:0.01%.

[0091] The binder used in step S2 is acrylic resin; the penetrant used is fatty alcohol polyoxyethylene ether; the crosslinking agent used is polyfunctional aziridine crosslinking agent.

[0092] Comparative Example 1

[0093] The difference between this comparative example and Example 1 is that in step S2, there is no binder, and the zinc oxide suspension, penetrant and crosslinking agent are mixed according to the mass ratio of 98%:1%:1%.

[0094] Comparative Example 2

[0095] The difference between this comparative example and Example 8 is that in step S2, a 20% quaternary ammonium salt solution is added, and the zinc oxide suspension, binder, penetrant and crosslinking agent are mixed according to the mass ratio of 92%:5%:1%:1%:1%.

[0096] The finishing agent prepared according to this formula will solidify after being placed.

[0097] The zinc oxide antibacterial finishing agents prepared in Examples 1-8 and Comparative Example 1 were mixed with water at a ratio of 5% to obtain an antibacterial finishing agent with a mass concentration of 5%. The bath ratio was 1:15 - 1:20. The post-finishing process was to soak for 30 min, and the expression rate was about 100%. First, dry at 80 °C for 40 - 50 min, then perform high-temperature baking at 130 °C for 5 - 6 min. After drying, samples 1 - 9 of antibacterial fabrics were obtained. An untreated polyester textile was taken as a blank sample for comparison.

[0098] According to the provisions of the national standard of the People's Republic of China GB8629-2001 "Domestic Washing and Drying Procedures for Textile Testing", a Type B agitator washing machine and washing program 8B were selected to perform washing treatments on the antibacterial-treated and untreated polyester fabrics respectively. Each specimen was washed 10 times, 30 times, and 50 times, and the antibacterial properties of the specimens after washing were measured.

[0099] Antibacterial test method: GB / T 20944.3-2008 Evaluation of Antibacterial Properties of Textiles - Part 3: Oscillation Method.

[0100] The test strains were bacteria: Staphylococcus aureus (ATCC6538), Escherichia coli (ATCC 25922), and fungi: Candida albicans (ATCC10231). The test results were recorded in Table 1:

[0101] Table 1 Test Results of Antibacterial Properties

[0102]

[0103] As can be seen from the data in Table 1, the antibacterial rates of the fabrics treated with the zinc oxide antibacterial finishing agents prepared in Examples 1-8 against three representative strains are all higher than 99% under the unwashed condition, and the antibacterial rate can still reach more than 90% after 50 washes. This indicates that the zinc oxide antibacterial finishing agent prepared in the present invention has good bonding fastness with the fabric and has efficient and long-lasting antibacterial effects. For the antibacterial fabric treated in Comparative Example 1 without an adhesive, the antibacterial performance significantly decreases after multiple washes.

[0104] Finally, 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 them; although the present invention has been described in detail with reference to the foregoing embodiments, those of ordinary skill in the art should understand that they can still modify the technical solutions described in the foregoing embodiments, or perform equivalent replacements on some or all of the technical features; and 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 preparation method of a zinc oxide antibacterial finishing agent, characterized in that, It includes the following steps: S1. Prepare zinc oxide suspension: Add zinc oxide powder and wetting agent to part of water, stir for 0.5 - 1 h, then add dispersion stabilizer and stir for 0.5 - 1 h. After that, add pH regulator and stir thoroughly, then add the remaining water and stir thoroughly. Further, grind and disperse at the first stirring rate for 2 h, then grind and disperse at the second stirring rate for 13 - 14 h. Finally, add defoamer and grind and disperse at the third stirring rate for 0.5 h to obtain the zinc oxide suspension; S2. Prepare zinc oxide antibacterial finishing agent: Stir the prepared zinc oxide suspension, binder, penetrant and crosslinking agent thoroughly at the third stirring rate; In step S1: The particle size of the zinc oxide powder is 1 - 50 μm; In step S1: The zinc oxide powder accounts for 10 - 35% of the total mass of the suspension; the wetting agent accounts for 0.1 - 1% of the mass of the zinc oxide powder; the dispersion stabilizer accounts for 1 - 15% of the mass of the zinc oxide powder; the pH regulator accounts for 0.1 - 3% of the total mass of the suspension, and it is diluted by 10 - 30% in advance before addition; the defoamer accounts for 0.01 - 0.1% of the total mass of the suspension; the rest is water; In step S1: The wetting agent is fatty alcohol polyoxyethylene ether; the dispersion stabilizer is one or more of polyacrylate, sodium polycarboxylate, ammonium polycarboxylate, dodecylbenzenesulfonate; the pH regulator is one or more of citric acid, oxalic acid, sodium citrate, potassium citrate, sodium hydroxide; the defoamer is one or more of fatty acid, fatty acid ester, phosphate ester, polyether modified silicone; The first stirring rate is 300 - 400 r / min, the second stirring rate is 600 - 800 r / min, and the third stirring rate is 100 - 200 r / min.

2. The preparation method of a zinc oxide antibacterial finishing agent as described in claim 1, characterized in that, In step S2: By mass percentage, it includes: 80 - 98% of zinc oxide suspension, 0.5 - 15% of binder, 0.5 - 5% of penetrant, 0.5 - 5% of crosslinking agent.

3. The preparation method of a zinc oxide antibacterial finishing agent according to claim 1, characterized in that, In step S2: The binder is one or more of acrylic resin, polyvinyl alcohol resin, waterborne polyurethane resin, carboxymethyl cellulose; the penetrant is one or more of secondary alkyl sulfonate, α-olefin sulfonate, alkyl naphthalene sulfonate, alkyl succinate sulfonate, sodium aminosulfonate, fatty alcohol polyoxyethylene ether; the crosslinking agent is one or more of polyfunctional aziridine crosslinking agent, isocyanate crosslinking agent, polyaziridine crosslinking agent, aziridine modified isocyanate crosslinking agent.

4. Use of a zinc oxide antibacterial finishing agent prepared by the preparation method of the zinc oxide antibacterial finishing agent according to any one of claims 1-3 in textile products, characterized in that, Applied to the after-finishing of textile fabrics, add zinc oxide antibacterial finishing agent according to the proportion of 4 - 10%, the bath ratio is 1:10 - 1:20, and then carry out padding, pre-drying and baking treatments to obtain the fabric containing zinc oxide antibacterial finishing agent.

Citation Information

Patent Citations

  • Composite antibiotic finishing agent for textiles

    CN105019236A

  • Process for preparing textile nano function finishing agent

    CN1632214A