Antibacterial yarn and preparation process thereof

By coating micron-sized tetrapod-shaped zinc oxide with nano-tourmaline and modifying it with piperazine and phenolic hydroxyl compounds, the problem of insufficient durability of antibacterial yarn was solved, and the washing resistance and durability of the antibacterial yarn were improved.

CN120797410APending Publication Date: 2025-10-17XINXIANG HUALU TECHNOLOGY CO LTD
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Patent Information

Application Number
CN202510893446.X
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-06-30
Publication Date
2025-10-17

AI Technical Summary

Technical Problem

In the prior art, the antibacterial yarn prepared by using tetrapod-shaped zinc oxide as an antibacterial agent has poor durability.

Method used

Nano-scale tourmaline coated micron-sized tetrapod-shaped zinc oxide is used as an antibacterial agent, and combined with a modified antibacterial agent containing a piperazine group and a phenolic hydroxyl group to prepare an antibacterial yarn. The coating is performed by mechanical stirring or ball milling to optimize the combination of the active groups of the antibacterial agent with the cotton fiber.

Benefits of technology

The washing resistance and antibacterial durability of the antibacterial yarn are improved, and the persistence and stability of the antibacterial performance are enhanced.

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Abstract

The invention relates to the technical field of textiles, and provides an antibacterial yarn and a preparation process thereof. The antibacterial yarn comprises cotton fibers and Juncao fibers, the cotton fibers are treated through an antibacterial finishing agent, and the antibacterial finishing agent is prepared from, by mass, 1-8 parts of a compound modified antibacterial agent containing piperazinyl and phenolic hydroxyl, 0.5-1.5 parts of an antistatic agent, 1-5 parts of a thickening agent and 100 parts of water. An antibacterial agent in the compound modified antibacterial agent containing piperazinyl and phenolic hydroxyl is nanoscale tourmaline coated micron-sized tetrapod-like zinc oxide. By means of the technical scheme, the problem that in the prior art, tetrapod-like zinc oxide is adopted as an antibacterial agent to conduct antibacterial after-treatment on fabric, and the prepared antibacterial yarn is poor in durability is solved.
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Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of textiles, in particular to an antibacterial yarn and a preparation process thereof. BACKGROUND

[0002] With the progress of society and economic development, people's living standards are getting higher and higher, and consumer concepts are constantly updated and improved, paying more attention to healthy high-quality life, and sports scenes are becoming more and more diverse. The transmission probability of pathogens such as bacteria and viruses is also increasing. Among various transmission routes, textiles are one of the main carriers. Because of their porous and loose structure, they are easy to adsorb various impurities and become carriers of pathogens, which greatly increases the cross-infection rate of public environment.

[0003] At present, in order to improve the antibacterial effect of textiles, two methods are mainly used: one is to perform antibacterial finishing on fabrics that do not have antibacterial function themselves, and the other is to prepare fibers with antibacterial properties through fiber modification. Compared with the latter, the former has a simple processing technology, mainly by means of immersion adsorption, chemical reaction, coating and other ways to combine antibacterial components onto fabrics or fibers. It is more commonly used, but because the antibacterial components and fibers are not a whole, with the increase of the number of textile washing, the antibacterial components will gradually fall off, and the antibacterial durability is poor.

[0004] In order to obtain fabrics with better antibacterial durability, four-needle-shaped zinc oxide is used as an antibacterial agent to perform antibacterial finishing on fabrics. Because the multi-branch needle-shaped structure of four-needle-shaped zinc oxide can form stronger mechanical engagement with fibers, limiting the relative sliding, thereby improving the washing resistance of antibacterial fabrics, but with more and more washing times, the effect of antibacterial durability needs to be further improved. SUMMARY

[0005] The present application provides an antibacterial yarn and a preparation process thereof, which solves the problem of poor durability of the antibacterial yarn prepared by using four-needle-shaped zinc oxide as an antibacterial agent to perform antibacterial finishing on fabrics in the related art.

[0006] The technical scheme of the present application is as follows: An antibacterial yarn, comprising cotton fibers and reed fibers, the cotton fibers are treated with an antibacterial finishing agent, the raw materials of the antibacterial finishing agent include the following components by mass fraction: a compound modified antibacterial agent containing piperazine group and phenolic hydroxyl group 1-8 parts, an antistatic agent 0.5-1.5 parts, a thickening agent 1-5 parts, water 100 parts, and the antibacterial agent in the compound modified antibacterial agent containing piperazine group and phenolic hydroxyl group is nano-sized tourmaline coated micron-sized four-needle-shaped zinc oxide.

[0007] As a further technical solution, the mass ratio of the cotton fiber and the straw fiber is 35:65~50:50, for example, it can be 35:65, 37:63, 40:60, 42:58, 45:55, 47:53 or 50:50, but is not limited to the listed values, and other unlisted values in the value range are also applicable.

[0008] As a country with the largest chemical fiber production and fiber consumption market in the world, the green, low-carbon and high-quality development of the textile industry cannot be separated from the continuous development and improvement of the fiber industry. From the perspective of national economic development and industrial safety and sustainable development, the cellulose content of straw is high, the growth cycle is short, and the yield per mu is high. The clothes made of straw fiber can be naturally degraded, and there is no pollution to the environment after decomposition. The straw fiber technology "replaces wood with grass" opens up a new way for cellulose fiber raw materials. The development and production of straw fabric are highly consistent with the concept of national ecological civilization, and help the national ecological civilization construction. Straw fiber is a new type of regenerated cellulose fiber, which is the fifth largest natural fiber after cotton, hemp, wool and silk. It is a natural, green and environmentally friendly fiber with excellent natural antibacterial and antiviral properties. It can achieve the purpose of antibiosis by inhibiting or destroying the self-metabolism and reproduction of bacteria in the nutrient source, and can achieve the purpose of antiviral by inhibiting or destroying the virus from invading host cells. Moreover, straw fiber also has the characteristics of natural, durable, green and harmless, and can be blended with cotton, wool, hemp, silk and chemical fibers to produce various yarns for weaving or knitting. Preferably, it is blended with cotton fiber because cotton fiber has good moisture absorption, is not easy to produce static electricity, has soft and comfortable touch, and is natural, comfortable and breathable, and the fabric is durable and wearable.

[0009] In the present application, the antistatic agent can be any one or more conventional antistatic agents in the art, preferably polydiallyldimethylammonium chloride; the thickening agent can be any one or more conventional thickening agents in the art, for example, polyvinyl alcohol, polyvinylpyrrolidone, cellulose, etc., preferably hydroxyethyl cellulose.

[0010] As a further technical solution, the raw material for coating the micron-sized four-needle-shaped zinc oxide with the nano-sized tourmaline includes nano-sized tourmaline and micron-sized four-needle-shaped zinc oxide with a mass ratio of 1:99~10:90.

[0011] As a further technical solution, the preparation method of the micron-sized four-needle-shaped zinc oxide coated with the nano-sized tourmaline includes the following steps: mixing the nano-sized tourmaline and the micron-sized four-needle-shaped zinc oxide, and then coating to obtain the micron-sized four-needle-shaped zinc oxide coated with the nano-sized tourmaline.

[0012] In the present application, the coating can be carried out by mechanical stirring, grinding or ball milling, preferably ball milling.

[0013] As a further technical solution, the rotation speed of the ball mill is 200-500 rpm, for example, it can be 200 rpm, 250 rpm, 300 rpm, 350 rpm, 400 rpm, 450 rpm or 500 rpm, but not limited to the listed values, other values not listed in this range are also applicable.

[0014] As a further technical solution, the ball milling time is 1-3h, for example, it can be 1h, 1.2h, 1.5h, 2h, 2.5h, 2.8h or 3h, but not limited to the listed values, other values not listed in this range are also applicable.

[0015] As a further technical solution, the raw material of the compound containing piperazine group and phenolic hydroxyl group modified antibacterial agent includes a compound containing piperazine group and phenolic hydroxyl group and an antibacterial agent with a mass ratio of 1-2:100.

[0016] As a further technical solution, the preparation method of the compound containing piperazine group and phenolic hydroxyl group modified antibacterial agent includes the following steps: dissolving the compound containing piperazine group and phenolic hydroxyl group in the solvent, adding the antibacterial agent and stirring until uniform, drying to obtain the compound containing piperazine group and phenolic hydroxyl group modified antibacterial agent.

[0017] In the present application, the compound containing piperazine group and phenolic hydroxyl group can be any one or more compounds containing piperazine group and phenolic hydroxyl group, for example, it can be 4-(1-piperazinyl) phenol, 2-(1-piperazinyl) phenol, 3-(2-piperazine) phenol, preferably 4-(1-piperazinyl) phenol.

[0018] The present application also provides a preparation process of antibacterial yarn for preparing the antibacterial yarn, which comprises the following steps: S1, the cotton fiber is immersed in the finishing agent for padding, drying to obtain the cotton fiber; S2, the cotton fiber and the straw fiber are sequentially opened, mixed, cleaned, carded, drawn, roved, spun, formed and packaged to obtain the antibacterial yarn; The finishing agent is composed of an antibacterial finishing agent and water with a mass-volume ratio of 100g:1-1.2L.

[0019] In the application, FA006 type reciprocating grabber and FA103 type double shaft flow opener are adopted in the opening process, followed by FA028 type six-bin cotton mixer (TV425A type cotton conveying fan) for mixing, and FA109 type three-roller clearer and FA151 type micro-dust remover for clearing impurities; then FAl77A type feeding box and FA221B type carding machine (6-8 machines) x 2 groups are adopted for carding, while removing impurities and short fibers; FA326 type drawing frame is adopted for drawing and mixing evenly; then FA426 roving frame, FA506 spinning frame and №21C winding machine are sequentially adopted; finally, the package is obtained, that is, the antibacterial yarn.

[0020] The carding and combing unit adopts the process principle of "short process, low speed, light single weight, more loose and less beating, and combing instead of beating", to prevent the occurrence of the phenomenon of returning flowers. The speed of the beater of the grabber is 740 r / min, the running speed of the grabber trolley is appropriately increased, and the trolley running rate is not less than 90%. The carding machine adopts a carding needle beater, and the speed is controlled within 480 r / min to reduce fiber damage. The output speed of the carding machine is controlled within 60 m / min, the sliver weight is 18 g / 5 m, and the cotton web is free of cotton blocks, holes, cloud spots and broken edges.

[0021] The 2-way drawing and mixing adopt 6-way combination, and the process principle of "low speed, medium weight, heavy pressure" is adopted. The surface roller is treated with an anti-winding agent, the speed is 150 m / min, the head and tail of the first way are 18 g / 5 m and the tail of the last way is 16 g / 5 m, and the sliver unevenness is 3.2%. The roving adopts the process principle of "heavy pressure, large twist factor and small tension", the speed should not be too high, and the spindle speed is controlled within 700 r / min. The tension should not be too large to avoid accidental draft. The roving weight is 3.7 g / 10 m, the twist factor is 95, and the sliver unevenness is 4.5%. The spinning adopts heavy pressure process, the spindle speed is 13000 r / min, the twist factor is 380, and the sliver unevenness is 14.5%. Double-in and double-out horn mouths are adopted to ensure that the two rovings are normally fed and do not appear to be entangled. The special-shaped tube adopts an upper 6 mm and lower 2 mm suction port, and reducing the lower port distance is beneficial to reducing the twist triangle zone tension and reducing the broken ends. A 128 mesh grid ring is selected to improve the air permeability to prevent the grid ring from accumulating flowers. A non-treatment rubber roller is adopted, and the diameter is controlled to be larger to improve the holding force, improve the sliver, and reduce the broken ends. The winding speed is 700 m / s, and the twist joint strength is not less than 95% of the original yarn. The electric cleaning focuses on removing short and thick sections.

[0022] As a further technical solution, the padding nip is 85% to 95%, for example, it can be 85%, 90% or 95%, but it is not limited to the listed values, and other unlisted values within the value range are also applicable.

[0023] The working principle and beneficial effects of the application are: The compound containing piperazinyl and phenolic hydroxyl is used to modify the antibacterial agent in the application, wherein the antibacterial agent is micron-sized tourmaline coated micro-sized four-needle-shaped zinc oxide, and the antibacterial durability of the antibacterial yarn prepared by using the micro-sized four-needle-shaped zinc oxide as the antibacterial agent is improved. The reason is that the micro-sized four-needle-shaped zinc oxide is coated with the nano-sized tourmaline, and then modified by the compound containing piperazinyl and phenolic hydroxyl, the modification effect is better, more active groups can be introduced on the surface, and the force is generated with the -OH on the cotton fiber, and the fiber is connected into one, so that the antibacterial yarn has excellent washing resistance, and the effect of improving the durability of the antibacterial yarn is achieved. DETAILED DESCRIPTION

[0024] The technical solutions in the embodiments of the application will be clearly and completely described below with reference to the embodiments of the application. Obviously, the described embodiments are only part of the embodiments of the application, rather than all the embodiments. Based on the embodiments in the application, all other embodiments obtained by those skilled in the art without creative labor are within the scope of protection of the application.

[0025] The parameters of the raw materials in the following examples and comparative examples are as follows: The nano-sized tourmaline is nano-sized tourmaline powder, and the particle size is 100 nm; The micro-sized four-needle-shaped zinc oxide: the length of the needle-shaped body is 10-50 μm, and the diameter of the root of the needle-shaped body is 0.5-5 μm; The straw fiber: Xinxing Chemical Fiber 1.5D*38mm staple fiber, the moisture regain is 12-15%; The cotton fiber: 229 grade machine-harvested Xinjiang cotton, the breaking specific strength is >30 cN*tex, the micronaire value is A grade (3.7-4.2), the neps content is ≤12%, the impurity content is ≤2.5%, and the moisture regain is 8.5%. -1

[0026] A preparation process of an antibacterial yarn, comprising the following steps: S1, immersing the cotton fiber into the finishing agent composed of the antibacterial finishing agent and water in a mass / volume ratio of 100g:1L for padding, the padding rate is 90%, and drying to obtain the cotton fiber; S2, sequentially opening, mixing, removing impurities, carding, drawing, roving, spinning, forming and packaging the cotton fiber and the straw fiber to obtain the antibacterial yarn; ​The blending ratio of the cotton fiber and the microalgae fiber is 50:50; a FA006 reciprocating grabber and a FA103 double-axial-flow opener are used in the opening process, a FA028 six-bin cotton mixer (TV425A cotton conveying fan) is used for mixing, and a FA109 three-roller clearer and a FA151 micro-dust remover are used for cleaning; a FA177A feeding box and a FA221B carding machine (6-8 machines) x 2 groups are used for carding; a FA326 drawing frame is used for drawing; a FA426 roving frame, a FA506 spinning frame, and a №21C winding machine are used for roving, spinning, and forming, respectively; the principle of "short process, low speed, light single weight, more loose and less beating, and combing instead of beating" is used in the blowing and carding combination to prevent the occurrence of the flower returning phenomenon. The speed of the grabber beater is 740 r / min, and the trolley running rate is 90%. The opening machine uses a carding needle beater, and the speed is 480 r / min. The output speed of the carding machine is 60 m / min, and the sliver weight is 18 g / 5 m.

[0027] The six-end drawing uses 6 ends of blending, and the principle of "low trolley speed, medium weight, and heavy pressure" is used. The skin roller is treated with an anti-winding agent, the speed is 150 m / min, the head-end and the end-end weight is 18 g / 5 m and 16 g / 5 m respectively, and the sliver unevenness is 3.2%. The roving uses the principle of "heavy pressure, large twist factor, and small tension", and the spindle speed is 700 r / min. The roving weight is 3.7 g / 10 m, the twist factor is 95, and the sliver unevenness is 4.5%. The spinning uses heavy pressure process, the spindle speed is 13000 r / min, the twist factor is 380, and the sliver unevenness is 14.5%. A double-in and double-out horn mouth is used to ensure the normal feeding of the two rovings, and the feeding process does not appear to be entangled. The special-shaped tube uses an upper 6 mm and lower 2 mm suction port, and reducing the lower port distance is beneficial to reducing the twist triangle area tension and reducing the broken ends. A 128 mesh grid ring is selected to improve the air permeability to prevent the grid ring from accumulating flowers. The winding speed is 700 m / s, and the twist joint strength is 95% of the original yarn.

[0028] The antibacterial finishing agent is prepared by the following method: Example 1 A1, nano-sized tourmaline and micron-sized four-needle-shaped zinc oxide are mixed in a mass ratio of 1:99, ball milled at 200 rpm for 3 h, and an antibacterial agent is obtained; A2, 4-(1-piperazinyl) phenol 2 parts are dissolved in 120 parts of ethanol, then 100 parts of the antibacterial agent are added and stirred at 800 rpm for 0.5 h, and then dried to obtain a modified antibacterial agent; A3, the modified antibacterial agent 8 parts is mixed with water 100 parts, then polydiallyldimethylammonium chloride 1.5 parts and hydroxyethyl cellulose 5 parts are added and uniformly mixed to obtain an antibacterial finishing agent.

[0029] Example 2 A1, nanoscale tourmaline and micron-sized tetrapod-shaped zinc oxide were mixed in a mass ratio of 1:9, then ball-milled at 500 rpm for 1 h to obtain an antibacterial agent; A2, 4-(1-piperazinyl) phenol 1.5 parts was dissolved in 120 parts of ethanol, then antibacterial agent 100 parts was added and stirred at 600 rpm for 1 h, and dried to obtain a modified antibacterial agent; A3, the modified antibacterial agent 8 parts was mixed with water 100 parts, then polydiallyldimethylammonium chloride 1.5 parts and hydroxyethyl cellulose 5 parts were added and uniformly mixed to obtain an antibacterial finishing agent.

[0030] Example 3 A1, nanoscale tourmaline and micron-sized tetrapod-shaped zinc oxide were mixed in a mass ratio of 1:9, then ball-milled at 500 rpm for 1 h to obtain an antibacterial agent; A2, 4-(1-piperazinyl) phenol 1.5 parts was dissolved in 120 parts of ethanol, then antibacterial agent 100 parts was added and stirred at 600 rpm for 1 h, and dried to obtain a modified antibacterial agent; A3, the modified antibacterial agent 8 parts was mixed with water 100 parts, then polydiallyldimethylammonium chloride 1.5 parts and hydroxyethyl cellulose 5 parts were added and uniformly mixed to obtain an antibacterial finishing agent.

[0031] Comparative Example 1 Micron-sized tetrapod-shaped zinc oxide 8 parts was mixed with water 100 parts, then polydiallyldimethylammonium chloride 1.5 parts and hydroxyethyl cellulose 5 parts were added and uniformly mixed to obtain an antibacterial finishing agent.

[0032] Comparative Example 2 Nanoscale tourmaline 0.4 parts and micron-sized tetrapod-shaped zinc oxide 7.6 parts were mixed with water 100 parts, then polydiallyldimethylammonium chloride 1.5 parts and hydroxyethyl cellulose 5 parts were added and uniformly mixed to obtain an antibacterial finishing agent.

[0033] Comparative Example 3 A1, 4-(1-piperazinyl) phenol 1.5 parts was dissolved in 120 parts of ethanol, then micron-sized tetrapod-shaped zinc oxide 100 parts was added and stirred at 600 rpm for 1 h, and dried to obtain a modified antibacterial agent; A2, the modified antibacterial agent 8 parts was mixed with water 100 parts, then polydiallyldimethylammonium chloride 1.5 parts and hydroxyethyl cellulose 5 parts were added and uniformly mixed to obtain an antibacterial finishing agent.

[0034] After the antibacterial yarns obtained in Examples 1 to 3 and Comparative Examples 1 to 3 are knitted, the pre-washing antibacterial rate is tested according to the method in GB / T 20944.3-2008 "Evaluation of antibacterial properties of textiles Part 3: oscillation method", and the post-washing antibacterial rate is tested after being washed 100 times in a standard washing machine of type B in GB / T 8629-2017 "Textiles Household washing and drying procedures" 8B program, and the antibacterial rate retention is calculated according to the following formula: Antibacterial rate retention (%) = post-washing antibacterial rate ÷ pre-washing antibacterial rate × 100; The results are recorded in Table 1.

[0035] Table 1: Pre-washing antibacterial rate and antibacterial rate retention

[0036] As can be seen from Table 1, the antibacterial rate retention of the antibacterial yarn knitted products obtained in Examples 1 to 3 is higher than that of Comparative Examples 1 to 3, which shows that the micron-sized four-needle-shaped zinc oxide is first coated with nanoscale tourmaline, and then modified with a compound containing a piperazine group and a phenolic hydroxyl group, thereby improving the antibacterial durability of the antibacterial yarn.

[0037] The above is only a preferred embodiment of the present application, and is not intended to limit the present application, and any modification, equivalent replacement, improvement, etc. made within the spirit and principles of the present application shall be included in the protection scope of the present application.

Claims

1. An antibacterial yarn comprising cotton fiber and Juncao fiber, wherein the cotton fiber is treated with an antibacterial finishing agent, characterized in that: The raw materials of the antibacterial finishing agent include the following components in parts by mass: 1 to 8 parts of an antibacterial agent modified with a compound containing piperazine and phenolic hydroxyl groups, 0.5 to 1.5 parts of an antistatic agent, 1 to 5 parts of a thickener, and 100 parts of water. The antibacterial agent in the antibacterial agent modified with a compound containing piperazine and phenolic hydroxyl groups is nano-scale tourmaline-coated micron-scale tetrapod-shaped zinc oxide.

2. The antibacterial yarn according to claim 1, characterized in that: The raw materials for the nano-level tourmaline-coated micron-level tetrapod-shaped zinc oxide include nano-level tourmaline and micron-level tetrapod-shaped zinc oxide in a mass ratio of 1:99 to 10:

90.

3. The antibacterial yarn according to claim 2, characterized in that: The preparation method of nano-level tourmaline-coated micron-level tetrapod-shaped zinc oxide comprises the following steps: mixing nano-level tourmaline and micron-level tetrapod-shaped zinc oxide, and then coating to obtain nano-level tourmaline-coated micron-level tetrapod-shaped zinc oxide.

4. The antibacterial yarn according to claim 3, characterized in that: The coating is carried out by ball milling, with a rotation speed of 200-500 rpm and a time of 1-3 hours.

5. The antibacterial yarn according to claim 1, characterized in that: The raw materials of the antibacterial agent modified with a compound containing piperazine and phenolic hydroxyl groups include a compound containing piperazine and phenolic hydroxyl groups and an antibacterial agent in a mass ratio of 1 to 2:

100.

6. The antibacterial yarn according to claim 5, characterized in that: The compound containing a piperazinyl group and a phenolic hydroxyl group includes one or more of 4-(1-piperazinyl)phenol, 2-(1-piperazinyl)phenol, and 3-(2-piperazine)phenol.

7. The antibacterial yarn according to claim 6, characterized in that: The compound containing piperazinyl and phenolic hydroxyl group is 4-(1-piperazinyl)phenol.

8. The antibacterial yarn according to claim 5, characterized in that: The preparation method of the compound modified antibacterial agent containing piperazinyl and phenolic hydroxyl groups comprises the following steps: dissolving the compound containing piperazinyl and phenolic hydroxyl groups in a solvent, adding an antibacterial agent, stirring until uniform, and drying to obtain the compound modified antibacterial agent containing piperazinyl and phenolic hydroxyl groups.

9. A process for preparing antibacterial yarn, for preparing the antibacterial yarn according to any one of claims 1 to 8, characterized in that: The following steps are involved: S1, immersing the cotton fiber in a finishing agent, padding, and drying to obtain the cotton fiber; S2, sequentially opening, mixing, cleaning, carding, drawing, roving, spinning, forming, and packaging the cotton fiber and the mushroom grass fiber to obtain the antibacterial yarn; The finishing agent consists of an antibacterial finishing agent and water in a mass volume ratio of 100g:1-1.2L.

10. The process for preparing an antibacterial yarn according to claim 9, characterized in that: The rolling rate of the soaking and rolling is 85% to 95%.

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