CN-122013516-A - Novel method for preparing long-acting antibacterial fiber product based on silane coupling agent in-situ quaternization

CN122013516ACN 122013516 ACN122013516 ACN 122013516ACN-122013516-A

Abstract

The invention discloses a novel method for preparing a long-acting antibacterial fiber product based on in-situ quaternization of a silane coupling agent, which comprises the steps of firstly coupling and grafting amino silane to the surface of cellulose-based fiber or the product thereof, further, the quaternization of the amino group is realized by introducing halogenated long-chain alkane, so that a chemically bonded cationic molecular brush structure is formed on the surface of the fiber. The invention makes up the performance limitation of a single antibacterial mechanism by constructing a double-effect antibacterial mechanism with the synergy of quaternized cations and alkyl chains, and the prepared grafted antibacterial cellulose-based fiber or the product thereof has the characteristics of high efficiency, antibacterial property and long-acting stability. The invention has simple process and mild condition, is suitable for cellulose-based fibers such as cotton, hemp and the like and products thereof, can realize long-acting antibacterial function, and has good application prospect in the fields of medical textile, daily protection and the like.

Inventors

XU XIAOLING
HAN XIAOCHEN
QU XI
ZHOU ZUOWAN
LIU CONGWEN
RAN QIANG
YU WENXUAN
ZHAO YUJIE
LIANG PENG

Assignees

西南交通大学

Dates

Publication Date: 20260512
Application Date: 20260126

Claims (8)

1. The novel method for preparing the long-acting antibacterial fiber product based on the in-situ quaternization of the silane coupling agent is characterized by comprising the following steps: s1 pretreatment Pretreating an initial cellulose-based fiber or product to obtain a pretreated cellulose-based fiber or product; s2 grafting aminosilane coupling agent S21, dissolving an aminosilane coupling agent in an ethanol water solution, and stirring to obtain a silane coupling solution, wherein the aminosilane coupling agent is one or two of N, N-dimethyl-3-aminopropyl trimethoxy silane and N, N-diethyl-3-aminopropyl trimethoxy silane; S22, adding the pretreated cellulose-based fiber or product obtained in the step S1 into the silane coupling solution for soaking, and then heating for reaction to obtain a reacted fabric A; s23, cleaning and drying the fabric A after the reaction to obtain cellulose-based fibers or products grafted with the aminosilane coupling agent; s3 quaternization treatment S31, mixing absolute ethyl alcohol and halogenated alkane, and stirring to obtain alkane solution; s32, adding the cellulose-based fiber or product grafted with the aminosilane coupling agent obtained in the step S2 into the alkane solution for soaking, and then heating for reaction to obtain a reaction fabric B; And S33, cleaning and drying the reacted fabric B to obtain the grafted antibacterial cellulose-based fiber or product.
2. The novel method for preparing a long-acting antibacterial fiber product based on in-situ quaternization of a silane coupling agent as claimed in claim 1, wherein the mass ratio of the aminosilane coupling agent to the ethanol aqueous solution in the step S21 is 1:7-10.
3. The novel method for preparing a long-acting antibacterial fiber product based on in-situ quaternization of a silane coupling agent as claimed in claim 2, wherein the ethanol aqueous solution in the step S21 is prepared by mixing absolute ethanol and deionized water according to a volume ratio of 5-20:1.
4. The novel method for preparing the long-acting antibacterial fiber product based on the in-situ quaternization of the silane coupling agent, which is disclosed in claim 1, is characterized in that the mass ratio of the pretreated cellulose-based fiber or product to the silane coupling solution in the step S22 is 1-10:90, the soaking time in the step S22 is 30-120 min, and the heating reaction condition is that the temperature is 80-140 ℃ and the reaction is 15-45min.
5. The novel method for preparing a long-acting antibacterial fiber product based on in-situ quaternization of a silane coupling agent as claimed in claim 1, wherein the mass ratio of absolute ethyl alcohol to halogenated alkane in the step S31 is 7-10:1.
6. The novel method for preparing a long-acting antibacterial fiber product based on the silane coupling agent in-situ quaternization as claimed in claim 5, wherein the halogenated alkane in the step S31 is one or more of chlorobutane, chlorooctane, chlorododecane and chlorohexadecane.
7. The novel method for preparing the long-acting antibacterial fiber product based on the silane coupling agent in-situ quaternization as claimed in claim 1, wherein the mass ratio of the cellulose-based fiber or the product grafted with the aminosilane coupling agent to the alkane solution in the step S32 is 1-10:90, the soaking time in the step S32 is 1-3h, and the heating reaction condition is that the temperature is 80-140 ℃ and the reaction is 15-60min.
8. The novel process for preparing a long-acting antibacterial fiber product based on the in-situ quaternization of a silane coupling agent as claimed in claim 1, wherein the cleaning conditions in the step S23 and the step S33 are that absolute ethanol and deionized water are alternately cleaned for 3 to 5 times, and the drying temperature is 50 to 80 ℃.

Description

Novel method for preparing long-acting antibacterial fiber product based on silane coupling agent in-situ quaternization Technical Field The invention relates to a novel method for preparing a long-acting antibacterial fiber product based on in-situ quaternization of a silane coupling agent, belonging to the technical field of antibacterial materials. Background With the enhancement of environmental awareness and the rise of health concerns, there is an increasing demand for functional fiber products. In the daily use process of the fiber product, most fabrics can be in direct contact with human bodies, and common fibers and fiber products have no cleaning capability on microorganisms and metabolites thereof, sweat, sebum and other secretions secreted by skin, oxygen and moisture in air and heat emitted by human bodies provide ideal living environments for microorganisms such as bacteria and fungi, and the problem that the fiber product is polluted by microorganisms is easily caused. Microbial contamination of the fibrous product not only damages the performance of the fibrous product itself, but also poses a great threat to personal health and public health. Therefore, the improvement of the antibacterial performance of the fiber product is more and more paid attention to, and becomes an important development direction of the functional fiber product. Common antibacterial modification methods of fabrics mainly comprise surface coating, physical blending and grafting modification. Wherein the surface coating has a limited storage capacity of the antibacterial agent in the surface coating, and the coating has a falling risk, so that the antibacterial effect of the surface coating has timeliness, and the common nano antibacterial agent can also have cytotoxicity and other safety risks. The antibacterial agent added during physical blending is difficult to uniformly distribute in a matrix when used as an additive due to poor compatibility, low dispersibility and the like, so that the antibacterial agent with low surface content can cause unstable antibacterial performance, and the antibacterial component can also have the risk of decomposition and damage in the polymer processing process. The surface grafting modification technology is an effective strategy for endowing the fabric with durable long-acting antibacterial property, and the antibacterial components are fixed on the surface of the base material through chemical action, so that the cotton fabric has the advantages of improving the antibacterial long-acting property, the safety and the like of the cotton fabric. In the prior art, a path of firstly synthesizing an antibacterial agent and then carrying out surface grafting is mostly adopted. For example, patent CN119842070A polymerized a polycationic guanidine salt with a benzene-containing ring compound to provide a polycationAnd the patent CN113818249A synthesizes a reactive cationic antibacterial monomer through chitosan and methacryloyloxyethyl trimethyl ammonium chloride, and then performs antibacterial finishing on the fabric by adopting a rolling baking finishing method. In addition, patent CN119507213a utilizes propylene oxide modified polyhexamethylene guanidine hydrochloride to prepare a novel polymer-based antimicrobial agent, and is grafted on the fabric surface after mixing with an organic acid deodorant. However, these prior art solutions of first synthesizing an antimicrobial agent and then grafting it to the fabric surface suffer from the disadvantages of complex and cumbersome steps and long time consumption. In order to solve the problems, the invention adopts an aminosilane grafting and then in-situ quaternization method to form a chemically bonded cationic molecular brush structure on the surface of cellulose-based fiber or a product thereof. The modification process is different from the traditional complex process of firstly synthesizing a specific antibacterial agent and then grafting the specific antibacterial agent onto the fabric through multi-step reaction, the obvious simplification and the improvement of efficiency of the modification process are realized, the modification conditions are mild, the inherent performance of cellulose-based fibers or products thereof is maintained, and the problems of poor broad-spectrum antibacterial property, poor antibacterial durability and the like can be effectively solved through a double-effect antibacterial mechanism of synergy of quaternized cations and alkyl chains. Disclosure of Invention The invention provides a novel method for preparing a long-acting antibacterial fiber product based on in-situ quaternization of a silane coupling agent, which aims to solve the problems of complicated process steps, harsh reaction conditions, poor broad-spectrum antibacterial property, insufficient long-acting property and the like in the conventional fabric antibacterial modification technology. The method forms a chemically bonded cation molecul