METHOD FOR PREPARING ANTIMICROBIAL TREATMENT AGENT FOR TEXTILE

Abstract

The present invention provides a method for preparing an antimicrobial treatment agent for textiles, including steps of: (S1) providing substances of: (a) divalent copper ion salt; (b) ammonia water or ammonium salt; (c) an inorganic alkaline aqueous solution; (d) an organic substance of alcohols or carbohydrates containing only carbon, hydrogen and oxygen elements; (e) water; and (S2) mixing and ageing above solutions using alcohols or carbohydrates as a catalyst to form a compound of a copper ammonium complex. In the method for preparing an antimicrobial treatment agent for textiles of the present invention, the treatment agent does not contain a heavy metal or an organic element that may have toxicity, for example, nitrogen, phosphorus or sulfur, an alkaline material used for treating the textile does not contain a non-volatile or an organic amine compound, an organic substance such as alcohols or carbohydrates is skillfully used as a catalyst, and copper ions form a complex for transition, so that natural textile fibers are grafted to copper ions more tightly and have advantages of safety, environmental friendliness, scrub resistance, a high antibacterial effect and long life of service.

Claims

1. A method for preparing an antimicrobial treatment agent for a textile, wherein the method includes steps of: Step S1 providing below substances: (a) salt containing divalent copper ion; (b) ammonia water or ammonium salt; (c) an inorganic alkaline aqueous solution; (d) an organic substance of alcohols or carbohydrates containing only carbon, hydrogen and oxygen elements; and (e) water; Step S2 mixing and ageing the above substances using alcohol or carbohydrate as a catalyst to form a compound of a copper ammonium complex.

2. The method for preparing an antimicrobial treatment agent for a textile according to claim 1, wherein said ammonium salt includes one or more of below substances: ammonium chloride, ammonium nitrate, ammonium sulfate, ammonium citrate and ammonium acetate.

3. The method for preparing an antimicrobial treatment agent for a textile according to claim 1, wherein said inorganic alkaline aqueous solution includes an aqueous solution of one or more of below substances: sodium carbonate, sodium acetate, sodium hydroxide and potassium hydroxide.

4. The method for preparing an antimicrobial treatment agent for a textile according to claim 1, wherein said organic substance of alcohols or carbohydrates includes one or more of below substances: methanol, ethanol, propylene glycol, glycerol, butanol, polyethylene glycol, glucose, an oligosaccharide and polysaccharide.

5. The method for preparing an antimicrobial treatment agent for a textile according to claim 1, wherein one or more of the organic substance of alcohols or carbohydrates in the compound is selected as catalyst, so that copper ions and a textile have good binding fastness and an antibacterial property.

6. The method for preparing an antimicrobial treatment agent for a textile according to claim 1, wherein said salt containing divalent copper ion is copper sulfate, said inorganic alkaline aqueous solution is sodium hydroxide, said organic substances includes ethanol, glycerol, propylene glycol, polyethylene glycol, and glucose, the part and percentage of raw materials below are measured by weight, the textiles adopt cellulose fiber fabrics, chemical fiber fabrics, regenerated fabrics, protein fabrics, or the like, wherein cellulose fiber fabrics includes cellulose, chemical fiber, polyester cotton, nylon, spandex, acrylic fiber, viscose, tencel, silk, or the like, and raw materials of said antimicrobial treatment agent comprise 10.1 parts of 50% copper sulfate aqueous solution, 2.9 parts of 28% ammonium hydroxide, 0.1 parts of 10% sodium hydroxide aqueous solution, 0.3 parts of ethanol, 1 part of glycerol, 3 parts of propylene glycol, 1 part of polyethylene glycol, 1.6 parts of glucose, and 80 parts of water.

Description

DETAILED DESCRIPTION

[0022] Some embodiments of the present invention are described below. Unless otherwise specified, all fractions and percentages illustrated in the following specific embodiments are measured by weight.

Embodiment 1

[0023] 10.1 parts of copper sulfate (50%), 2.9 parts of ammonium hydroxide (28%), 0.1 parts of sodium hydroxide aqueous solution (10%), 0.3 parts of ethanol, 1 part of glycerol, 3 parts of propylene glycol, 1 part of polyethylene glycol, 1.6 parts of glucose, and 80 parts of water were taken.

[0024] Reagents of copper sulfate, ammonium hydroxide, sodium hydroxide, propylene glycol, glycerol, and polyethylene glycol were prepared respectively in the above mentioned ratio, each of above reagents were dissolved and aged for 10 hours separately, mixed, maintained at 30 C.-35 C., stirred, and further aged for 24 hours to obtain an antimicrobial treatment agent. Herein, ethanol, glycerol, propylene glycol, polyethylene glycol and glucose were in a ratio of 0.3:1:3:1:1.6, pre-mixed and purified for 1 hour to obtain an organic substance of alcohol as a catalyst to well stabilize copper ions for transition.

Embodiment 2

[0025] 10.1 parts of copper sulfate (50%), 2.9 parts of ammonium hydroxide (28%), 0.1 parts of sodium hydroxide aqueous solution (10%), 3 parts of ethanol, 3 part of glycerol, 4 parts of propylene glycol, 3 part of polyethylene glycol, 9.9 parts of glucose, and 64 parts of water were taken.

[0026] Reagents of copper sulfate, ammonium hydroxide, sodium hydroxide, propylene glycol, glycerol, and polyethylene glycol were prepared respectively in the above mentioned ratio, each of the reagents was dissolved and aged for 10 hours separately, mixed, maintained at 30 C.-35 C., stirred, and further aged for 24 hours to obtain an antimicrobial treatment agent. Herein, ethanol, glycerol, propylene glycol, polyethylene glycol and glucose were in a ratio of 3:1:5:1:9.9.

Embodiment 3

[0027] 10.1 parts of copper sulfate (50%), 2.9 parts of ammonium hydroxide (28%), 0.1 parts of sodium hydroxide aqueous solution (10%), 1.9 parts of ethanol, 3 part of glycerol, 20 parts of propylene glycol, 3 part of polyethylene glycol, 10 parts of glucose, and 49 parts of water were taken.

[0028] Reagents of copper sulfate, ammonium hydroxide, sodium hydroxide, propylene glycol, glycerol, and polyethylene glycol were prepared respectively in the above mentioned ratio, each of the reagents was dissolved and aged for 10 hours separately, mixed, maintained at 30 C.-35 C., stirred, and further aged for 24 hours to obtain an antimicrobial treatment agent. Herein, ethanol, glycerol, propylene glycol, polyethylene glycol and glucose were in a ratio of 1.9:3:20:3:10.

Embodiment 4

[0029] 10.1 parts of copper sulfate (50%), 4.8 parts of ammonium hydroxide (28%), 0.1 parts of sodium hydroxide aqueous solution (10%), 2 parts of ethanol, 3 part of glycerol, 13 parts of propylene glycol, 3 part of polyethylene glycol, 10 parts of glucose, and 54 parts of water were taken.

[0030] Reagents of copper sulfate, ammonium hydroxide, sodium hydroxide, propylene glycol, glycerol, and polyethylene glycol were respectively prepared. Each of the reagents was dissolved and aged for 10 hours separately, mixed, maintained at 30 C.-35 C., stirred, and further aged for 24 hours to obtain an antimicrobial treatment agent. Herein, ethanol, glycerol, propylene glycol, polyethylene glycol and glucose were in a ratio of 2:3:13:3:10.

[0031] Textiles can be treated with the antimicrobial treatment agent prepared by the method of the present invention include cellulose fiber fabrics, chemical fibers, renewable fibers, viscose and the like. Specific treatment processes include dipping, padding, spraying, coating, and foam coating processing. (1) Dipping: dipping can also be called as soaking. After pretreatment, dyeing and washing of the fabrics were completed, at room temperature or 40 C., the microbial treatment agent was added to a dyeing vat at room temperature and atmospheric pressure, the fabrics can be removed from the dyeing vat after the dyeing vat was kept therein for 10 minutes, and the fabrics were dehydrated and dried. (2) padding: after the fabrics were dyed, washed and dried, the microbial treatment agent was evenly applied to the fabrics via one dipping treatment and one rolling treatment under pressure of 1.8 kg-4 kg, followed by curing and drying at a drying temperature of 100 C.-150 C., so that the fabrics react with the microbial treatment agent, thereby completing processing of the fabrics with the microbial treatment agent. (3) spraying: spraying is used for special products that cannot be soaked or padded but can only be subjected to a spraying process such as filling with an atomizing nozzle, and after spraying, the special product was dried at drying temperature of 100 C.-150 C. (4) coating process: a required amount of agent that needs to be subjected to the coating process was mixed with coating slurry, and applied to surfaces of the fabrics, followed by drying for cross-linking. (5) foam coating: performing foam coating can save water, a foaming agent and the antimicrobial treatment agent were used to form foam, followed by scraping coating and drying at drying temperature of 100 C.-150 C., and this process can save a lot of water and reduce a waste of energy.

[0032] In the foregoing four examples, when a concentration of ammonium hydroxide in the antimicrobial treatment agent prepared by the method of the present invention is increased, bounding fastness during washing of the antimicrobial treatment agent and fabric decreases. Ammonium hydroxide was prepared at different concentrations, other conditions were kept unchanged, the fabrics were washed after being treated with 3% antimicrobial treatment agent, and an antibacterial rate against Staphylococcus aureus was measured. Results are shown in the following table:

TABLE-US-00001 Measured antibacterial rate Measured antibacterial rate Percentage of 28% against Staphylococcus aureus against Staphylococcus aureus ammonium hydroxide after 50 times of after 20 times of (percentage) washing (percentage) washing (percentage) 2.9% Greater than 99.9% Greater than 99.9% 9% 60% 99% 16% 30% 50%

[0033] In addition, using glucose as a catalyst facilitates washing fastness of the antimicrobial treatment agent and the fabrics, using different or combined catalysts facilitates washing fastness of a bound microbial treatment agent and fabric, other conditions were kept unchanged, the fabrics were washed after being treated with 3% antimicrobial treatment agent, and an antibacterial rate against Staphylococcus aureus was measured. Results are shown in the following table:

TABLE-US-00002 Measured antibacterial rate Measured antibacterial against Staphylococcus aureus rate against Staphylococcus aureus after 50 times of after 20 times of Different catalysts washing (percentage) washing (percentage) Glucose 60% 99% Glycerol 50% 96% Polyethylene glycol 60% 90% Glycerol, propylene 99.9%.sup. 99.9%.sup. glycol, ethanol, polyethylene glycol and glucose

[0034] The following treatment examples show treatment results of various fabrics with the antimicrobial treatment agent (Example 1) prepared by the method of the present invention, and comparison between fabric treatment performance of the antimicrobial treatment agent of the present invention and that of a treatment agent in the prior art.

[0035] Example 1: Taking treatment of cotton yarn as example, a dipping process was performed, an agent of 2% (o.w.f) was added to an auxiliary vat, and 2 kg of antibacterial agent was required for 100 kg of yarn.

TABLE-US-00003 Antimicrobial Silver ion Triclosan treatment antibacterial antibacterial agent of the agent agent present invention Processing Needed to heat to Needed to Room temperature, efficiency 50 C. and process heated to 60 C., maintained for for at least maintained for 10 minutes 1.5 hours 30 minutes Washability 20 times of 10 times of 50 times of (FZ/T73023) washing washing washing Inhibition zone Less than Greater than 0 5 mm 5 mm Antibacterial rate 60% 0 Greater than after 50 times of 99.9% against washing Staphylococcus aureus (GB/T20944.3) and Escherichia coli

[0036] Example 2: Socks, a knitted cotton fabric, an underwear, and a T-shirt fabric were subjected to a dipping process. An agent accounting for 2% (o.w.f) was added to an auxiliary vat, and 2 kg of antibacterial agent was required for 100 kg of fabric. The agent was added at room temperature (the room temperature in a factory was generally 35 C.-40 C.), and the temperature was maintained for 10 minutes.

TABLE-US-00004 Antimicrobial treatment agent of the present invention Washability (FZ/T73023) 50 times of washing Inhibition zone 0 Antibacterial rate after 50 Greater than 99.9% against times of washing (GB/T20944.3) Staphylococcus aureus and Escherichia coli

[0037] Example 3: A towel was subjected to a dipping process. An agent accounting for 2% (o.w.f) was added to an auxiliary vat, and 2 kg of antibacterial agent was required for 100 kg of fabrics. The agent was added at room temperature (the room temperature in a factory was generally 35 C.-40 C.), and the temperature was maintained for 10 minutes.

TABLE-US-00005 Antimicrobial Silver ion Silicone treatment antibacterial quaternary agent in the agent ammonium salt present invention Processing The dipping Needed to Room temperature, efficiency process failed and heat to 50 C., maintained for therefore, was maintained for 10 minutes unavailable, and only 30 minutes padding process could be performed, which was a limitation. Washability 20 times of 10 times of 50 times of (FZ/T73023) washing washing washing Inhibition zone Less than Greater than 0 5 mm 5 mm Antibacterial rate 60% 0 Greater than 99.9% after 50 times of against washing Staphylococcus aureus (GB/T20944.3) and Escherichia coli Appearance Towel was not Water No impact fluffy after absorption padding. affected

[0038] Example 4: Home fabrics such as cotton, viscose, polyester, nylon, and blended fabrics were subjected to a padding process. An agent accounting for 2% (o.w.f) of the fabrics was added, after a liquid retention ratio was calculated, the agent was configured at a concentration, in which 2 kg of antibacterial agent was required for 100 kg of fabrics. The fabrics were subjected to a padding process, drying, curing and finishing.

TABLE-US-00006 Antimicrobial treatment agent in the present invention Standard FZ/T73023-AAA 50 times of washing Inhibition zone 0 Antibacterial rate after Greater than 99.9% against 50 times of Staphylococcus aureus washing (GB/T20944.3) and Escherichia coli

[0039] Example 5: Sportswear fabrics such as cotton, viscose, polyester and nylon were subjected to a padding process. An agent accounting for 2% (o.w.f) of the fabric was added, after a liquid retention ratio was calculated, the agent was configured at a concentration, i.e., 2 kg of antibacterial agent was required for 100 kg of fabric. The fabric was subjected to a padding process, drying, curing and finishing.

[0040] Test: After 50 times of washing, both antibacterial rates of Staphylococcus aureus and Escherichia coli were 99%.

[0041] Example 6: Work cloth fabrics were subjected to a padding process. For example, cotton, viscose, polyester and nylon were subjected to a padding process. An agent accounting for 2% (o.w.f) of the fabric was added, after a liquid retention ratio was calculated, the agent was configured at a concentration. That is, 2 kg of antibacterial agent was required for 100 kg of fabric. The fabric was subjected to a padding process, drying, curing and finishing.

[0042] Test: After 50 times of washing, both antibacterial rates of Staphylococcus aureus and Klebsiella pneumoniae tested according to AATCC100-2019 were 99%.

[0043] Example 7: Knitted fabrics for respirators were subjected to a padding process. An agent accounting for 2% (o.w.f) was added to an auxiliary vat, and 2 kg of antibacterial agent was required for 100 kg of fabric. The agent was added at room temperature (room temperature in a factory was generally 35 C.-40 C.), and the temperature was maintained for 10 minutes. The respirator was removed from the vat, followed by dehydration, drying, padding and three-proofing (water repellency, oil repellency and antifouling), and the antibacterial and three-proofing functions were completed.

[0044] Test: An antibacterial effect was measured according to AATCC135. After 30 times of washing, both antibacterial rates of Staphylococcus aureus and Klebsiella pneumoniae tested according to AATCC100-2019 were 99%.

[0045] Three-proofing effects: water repellency scores were 100 points before washing, and points after 30 times of washing. Oil repellency was level 5 before oil washing, and level 3.5 after oil washing.

[0046] This example resolved a problem that tens thousand meter large-scale production process cannot be achieved due to a conflict between antibacterial and three-proofing treatments in the past. In addition, the antibacterial treatment was completed in the vat without increasing costs for a factory. This example also resolved a problem that the antibacterial and three-proofing treatments required two curing treatments in the past, which causes a waste of energy and low production efficiency.

[0047] Example 8: Shirt fabrics were subjected to a padding process. For example, cotton, viscose, polyester and nylon were subjected to a padding process. An agent accounting for 2% (o.w.f) of the fabrics was added, after a liquid retention ratio was calculated, the agent was configured at the calculated concentration, that is, 2 kg of antibacterial agent was required for 100 kg of fabric. The fabric was subjected to a padding process, drying, curing and finishing.

[0048] Test: After 50 times of washing, both antibacterial rates of Staphylococcus aureus and Klebsiella pneumoniae tested according to AATCC100-2019 were 99%.

[0049] In this example, shirts were mostly white, a silver ion antibacterial agent was used in the past, the fabrics are easy to turn yellow during storage, the triclosan antibacterial agent has a safety problem, and washability cannot be achieved via a silicone quaternary ammonium salt antibacterial agent. After the treatment with the antimicrobial treatment agent of the present invention, a color hardly changed after storage, no antibacterial agent remained, and washability could be 50 times of washing.

[0050] Example 9: Jeans fabrics were subjected to a padding process. Components such as cotton, viscose, polyester and nylon were subjected to a padding process. An agent accounting for 2% (o.w.f) of the fabric was added, after a liquid retention ratio was calculated, the agent was configured at the calculated concentration, that is, 2 kg of antibacterial agent was required for 100 kg of fabrics. The fabrics were subjected to a padding process, drying, curing and finishing. The antimicrobial treatment agent may also be applied when jeans yarns were starched, and added together with yarn starch.

[0051] Test: After 50 times of washing, both antibacterial rates of Staphylococcus aureus and Klebsiella pneumoniae tested according to ISO20743-2013 were 99%.

[0052] The present invention resolved a problem of antibacterial failure when the antibacterial agent was mixed with indigo dyes and sulfur dyes in the yarn, and also resolved a problem of a lack of an antibacterial effect because 80% of the antibacterial agent fell off after the jeans fabric was washed with an enzyme.

[0053] Example 10: Gauze and rag fabrics. An agent accounting for 2% (o.w.f) of the gauze was added, and 2 kg of antibacterial agent was required for 100 kg of the gauze fabrics. After starch slurry was boiled, the antibacterial agent was directly added to the boiled starch slurry, and the gauze was subjected to padding, drying and finishing.

[0054] Test: After 50 times of washing, all antibacterial rates of Staphylococcus aureus, Escherichia coli and Candida albicans tested according to FZ/T73023-AAA were greater than 99%.

[0055] This example resolved a problem that no antibacterial agent could be used in the same bath with starch slurry in the past, which induces high process costs because padding and drying needs to be performed twice. The present invention reduces energy consumption.

[0056] Example 11: For filling of short fibers, a spraying process was performed, an agent accounting for 2% (o.w.f) of the gauze was added, and 2 kg of antibacterial agent was required for 100 kg of the short fibers. After a spraying rate was calculated, the required agent was configured in a batching tank, that is, 2 kg of antibacterial agent was required for 100 kg of the short fibers. The short fibers were subjected to spraying and drying.

[0057] Example 12: Dyeing of cotton fibers. An agent accounting for 2% (o.w.f) was added to an auxiliary vat of the dyeing vat, and 2 kg of antibacterial agent was required for 100 kg of fibers. The agent was added at room temperature (room temperature in a factory was generally 35 C.-40 C.), and the temperature was maintained for 10 minutes.

[0058] After 50 times of washing, all antibacterial rates of Staphylococcus aureus, Escherichia coli and Candida albicans tested according to FZ/T73023-AAA were greater than 99%.

[0059] This example resolved an antibacterial problem of cotton fibers. In the past, an antibacterial effect was easily unfulfilled and unstable when an antibacterial process was performed on the fibers. Only polyester-cotton blends could be used to achieve the antibacterial effect on polyester fibers, and the antibacterial process was not performed on cotton fibers. In the present invention, using 100% treated antibacterial fibers or adding 50% non-antibacterial fibers can achieve good antibacterial performance Starting a treatment from the fibers reduced a need to deliver the fabrics to a dyeing factory. After the fibers were treated, various finished products could be produced by spinning, thereby reducing transportation and energy consumption.

[0060] Example 13: Polar fleece fabrics in outdoor clothing. An agent accounting for 2% (o.w.f) was added to an auxiliary vat, and 2 kg of antibacterial agent was required for 100 kg of fabric. The agent was added at room temperature (room temperature in a factory was generally 35 C.-40 C.), and the temperature was maintained for 10 minutes.

TABLE-US-00007 Antimicrobial treatment agent of the present invention After 10 times 99.9% against Staphylococcus aureus of washing measured according to AATCC100-2019

[0061] This example resolved a problem that the antibacterial agent could only be used in a padding process in the past, which made the polar fleece fabric difficult to dry and required more than twice amount of energy because the polar fleece fabric was too thick. This example also resolved a problem that there was no batching tank on drying equipment of some polar fleece fabric factories and no additional function could be completed.

[0062] Although the present invention has been disclosed above through preferred embodiments, the embodiments are not intended to limit the present invention. Any equivalent changes or modifications made without departing from the spirit and scope of the present invention shall also fall within the protection scope of the present invention. Therefore, the protection scope of the present invention should be based on content defined in claims of the present application.