CN115976829A - Azo modified graphene, antibacterial and deodorant textile and preparation method thereof - Google Patents

Azo modified graphene, antibacterial and deodorant textile and preparation method thereof Download PDF

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Publication number
CN115976829A
CN115976829A CN202310024690.3A CN202310024690A CN115976829A CN 115976829 A CN115976829 A CN 115976829A CN 202310024690 A CN202310024690 A CN 202310024690A CN 115976829 A CN115976829 A CN 115976829A
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fabric
azo
negative pressure
graphene
modified graphene
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李义春
王进美
张琪
骆婉茹
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Zhejiang New Material Technology Co ltd
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Zhejiang New Material Technology Co ltd
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    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02ATECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
    • Y02A50/00TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
    • Y02A50/30Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change

Abstract

The invention relates to the technical field of material preparation, in particular to azo modified graphene, an antibacterial deodorizing textile and a preparation method thereof. The method comprises the following steps of carrying out diazo coupling reaction on 10-20 parts of graphene particles with the particle size of 0.1-0.2 micrometer, 6-8 parts of 2-bromoisobutyryl bromide, 15-25 parts of modified grafted polyethyl methacrylate and 1-2 parts of 4-cyanoaniline diazonium salt to obtain a graphene material with the surface grafted with azo polymer; then adding 3-5 parts of potassium phosphate and 5 parts of calcium carbonate; mixing the above components at 60-80 deg.C in sealed environment. The azo modified graphene material is adopted, so that the fabric has excellent antibacterial and deodorant properties, antiviral and far infrared properties, and the antibacterial and deodorant effects are lasting.

Description

Azo modified graphene, antibacterial and deodorant textile and preparation method thereof
Technical Field
The invention relates to the technical field of material preparation, in particular to azo modified graphene, an antibacterial deodorizing textile and a preparation method thereof.
Background
Graphene is a honeycomb two-dimensional nano material formed by tightly stacking carbon atoms, and has great application potential in various fields by virtue of a series of unique properties such as super-large specific surface area, high electrical conductivity, thermal conductivity and high strength. In order to fully utilize the excellent performance of graphene, the application range of graphene materials is increased by optimizing and modifying the graphene materials.
With the increasing awareness of people on life safety, health protection and ecological environmental protection concepts are widely concerned in the consumer market, and the requirements of textiles with antibacterial protection function are gradually increased, so that people not only need to wear comfortable healthy and environmental-friendly clothes, but also need to have functional fabrics for environmental changes, especially antibacterial performance, for the fabric to be taken.
The existing textile fabric is mostly woven by bamboo charcoal and other antibacterial and deodorant fibers in the textile, so that the textile has certain antibacterial and deodorant performances, but the preparation process of bamboo charcoal and other antibacterial and deodorant fiber fabric is complex, the antibacterial and deodorant performance of the material is controllable and limited from the preparation of antibacterial textile raw materials to the application, the production and application links are many, the novel textile material and the production are easy to operate and control, the cost is controlled, and the performance is improved. The production difficulty is high, and the large-scale application of the azo modified graphene on textile fabrics is limited, so that the azo modified graphene-based antibacterial deodorizing textile and the preparation method thereof are needed, and the antibacterial and deodorizing capabilities of the textile are guaranteed on the premise of simplifying the production process.
Disclosure of Invention
The invention aims to provide azo modified graphene, an antibacterial deodorizing textile and a preparation method thereof, and aims to solve the problems in the background art.
To achieve the above object, in one aspect, the present invention provides an azo-modified graphene, including:
10-20 parts of graphene particles with the particle size of 0.1-0.2 micrometer, 6-8 parts of 2-bromoisobutyryl bromide, 15-25 parts of modified grafted polyethyl methacrylate and 1-2 parts of 4-cyanoaniline diazonium salt, and performing diazo coupling reaction to obtain the graphene material with the surface grafted with the azo polymer; then adding 3-5 parts of potassium phosphate and 5 parts of calcium carbonate;
mixing the above components at 60-80 deg.C in sealed environment.
The functional group with hydroxyl reacts with 2-bromoisobutyryl bromide to prepare the initiator with atom transfer radical polymerization on the surface, the initiator is used for initiating the atom transfer radical polymerization of monomer alkene-methyl acrylate copolymer, and the in-situ polymerization is carried out on the surface of graphene to obtain modified grafted poly (ethyl methacrylate); carrying out diazo coupling reaction on the modified grafted polyethylmethacrylate and 4-cyanoaniline diazonium salt to obtain the graphene material with the surface grafted with the azo polymer, and improving antibacterial, far infrared and adhesive force by potassium phosphate and calcium carbonate.
As a further improvement of the technical scheme, the water content of the mixed composition is between 15 and 20 percent.
The water content is controlled by controlling the temperature and stirring, so that the overall performance of the composition is stable, and the subsequent process is facilitated.
The invention also discloses an antibacterial and deodorant textile, wherein the graphene layer of the fabric is formed by using the graphene material, and the fabric treated by the vacuum atomization negative pressure adsorption method comprises a fabric layer and the graphene layer coated on the surface of the fabric layer.
The invention also discloses a preparation method of the antibacterial and deodorant textile based on the azo modified graphene, which uses the graphene material; the method comprises the following steps:
s1: preparing an azo modified graphene material;
s2: compounding an azo modified graphene material and a titanium dioxide photocatalytic nano-structure material to prepare a finishing agent, and adding distilled water into the finishing agent for dilution;
s3: spraying the finishing agent onto the fabric by a vacuum atomization negative pressure adsorption method;
s4: and (3) feeding the fabric into a drying chamber, drying the fabric, and shaping at a high temperature of 180-200 ℃ for 2-3 s.
As a further improvement of the technical solution, in S1, the preparation method of the azo-modified graphene material is as follows:
s1.1, preparing graphene oxide by a chemical method, and reducing the graphene oxide by hydrazine hydrate to obtain reduced graphene oxide;
s1.2, grafting a functional group with hydroxyl on the surface of the reduced graphene oxide through diazo addition reaction;
s1.3, reacting a functional group with hydroxyl with 2-bromine isobutyryl bromide through a Schn-Baumann reaction to prepare a polymerization initiator with atom transfer radical on the surface;
s1.4, initiating an atom transfer radical polymerization reaction of a monomer alkene-methyl acrylate copolymer by using an initiator, and carrying out in-situ polymerization on the surface of graphene to obtain modified grafted polyethyl methacrylate;
s1.5, carrying out diazo coupling reaction on the modified grafted polyethylmethacrylate and 4-cyananiline diazonium salt to obtain the graphene material with the surface grafted with the azo polymer.
As a further improvement of the technical scheme, in S2, the azo-modified graphene material and the titanium dioxide photocatalytic nanostructure material are compounded in a ratio of 1-2; and adding distilled water into the finishing agent obtained by compounding, diluting the finishing agent and the distilled water according to a ratio of 1.
As a further improvement of the technical solution, in S3, the vacuum atomization negative pressure adsorption method specifically includes:
s3.1, conveying the fabric by adopting a negative pressure roller in a vacuum spraying chamber;
s3.2, in the process of conveying the fabric through the negative pressure roller, the surface of the fabric is atomized and sprayed in a multi-surface spraying mode at the flow rate of 12-15mL/min under the air pressure of 0.5-0.7Mpa, so that the surface tension of finishing agent liquid is broken under the action of pressure to be changed into fine aerial fog with the diameter of less than 3 mu m;
s3.3, sending the sprayed fabric into a drying chamber, and carrying out high-temperature shaping on the fabric at 180-200 ℃ for 2-3S;
and S3.4, feeding the sprayed wet fabric into a heat setting machine, and quickly cooling the fabric to room temperature within 2-3S before the fabric leaves the negative pressure roller conveyor after the fabric surface is heated to the setting temperature within 2-3S.
As a further improvement of the technical scheme, in S3.1, the upper surface and the lower surface of the fabric are both provided with spray nozzles, and the distance between each spray nozzle and the surface of the fabric is 1.2-1.6m; negative pressure is controlled by the induced draft fan in the negative pressure cylinder, sets up the air intake of induced draft fan on the negative pressure cylinder surface, and the air intake is laminated with the fabric, will spray the finishing agent that the mouth sprayed and lead to the fabric surface through the negative pressure cylinder.
As a further improvement of the technical scheme, in S3.4, the fabric is placed in a high-temperature environment of 180-200 ℃ in a tension state; the negative pressure rollers are arranged along the upper surface and the lower surface of the fabric in a staggered mode, the number of the negative pressure rollers distributed up and down per meter of the fabric and the adsorption force of each negative pressure roller are configured to enable the surface tension of the fabric to be 85-95mN/m; the number of the negative pressure rollers distributed up and down per meter of fabric is 3-4, and the value of the adsorption force is 6-10Pa.
As a further improvement of the technical scheme, the spray nozzles are arranged above and below the fabric in pairs, one spray nozzle is connected with a positive electrode, and the other spray nozzle is connected with a negative electrode, so that the sprayed and atomized finishing agent contains charged particles.
Compared with the prior art, the invention has the beneficial effects that:
the azo modified graphene material is adopted, so that the fabric has excellent antibacterial and deodorizing performances, antiviral performance and far infrared performance.
The finishing agent is formed by compounding an azo modified graphene material and a titanium dioxide photocatalysis nano-structure material, and the fabric has excellent antibacterial and deodorant properties and lasting antibacterial and deodorant effects by atomizing, spraying, drying and high-temperature setting through a vacuum atomization negative pressure adsorption method.
Drawings
FIG. 1 is a flow diagram of a textile manufacturing process of example 1;
FIG. 2 is a schematic drawing showing the results of the shower chamber of example 1 in plan view;
figure 3 is a plan view of the fabric of example 1.
The various reference numbers in the figures mean:
1. a spray chamber; 101. a shower head; 102. a negative pressure roller;
2. a fabric; 201. a fabric layer; 202. a graphene layer.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The embodiment provides an azo modified graphene, which includes:
10-20 parts of graphene particles with the particle size of 0.1-0.2 micrometer, 6-8 parts of 2-bromoisobutyryl bromide, 15-25 parts of modified grafted polyethyl methacrylate and 1-2 parts of 4-cyanoaniline diazonium salt to perform diazo coupling reaction to obtain a graphene material with the surface grafted with azo polymer; then adding 3-5 parts of potassium phosphate and 5 parts of calcium carbonate;
mixing the above components at 60-80 deg.C in sealed environment.
Preferably, the water content of the blended composition should be between 15-20%.
As shown in fig. 3, in the antibacterial deodorizing textile according to this embodiment, the graphene layer of the fabric is formed by using the graphene material, and the fabric 2 treated by the vacuum atomization negative pressure adsorption method includes a fabric layer 201 and a graphene layer 202 coated on the surface of the fabric layer 201.
Referring to fig. 1, a preparation method of an antibacterial and deodorant textile based on azo-modified graphene in this embodiment includes the following steps:
s1: preparing an azo modified graphene material;
the preparation method of the azo modified graphene material comprises the following steps:
s1.1, preparing graphene oxide by a chemical method, and reducing the graphene oxide by hydrazine hydrate to obtain reduced graphene oxide;
s1.2, grafting a functional group with hydroxyl on the surface of the reduced graphene oxide through diazo addition reaction;
s1.3, reacting a functional group with hydroxyl with 2-bromine isobutyryl bromide through a Schnutten-Baumann reaction to prepare a polymerization initiator with atom transfer radical on the surface;
s1.4, initiating an atom transfer radical polymerization reaction of a monomer alkene-methyl acrylate copolymer by using an initiator, and carrying out in-situ polymerization on the surface of graphene to obtain modified grafted polyethyl methacrylate;
s1.5, carrying out diazo coupling reaction on the modified grafted polyethylmethacrylate and 4-cyananiline diazonium salt to obtain a graphene material with the surface grafted with an azo polymer; the dispersibility of the azo modified graphene in the solvent is greatly improved compared with that of the graphene, a stable dispersion liquid can be formed in the organic solvent, the azo modified graphene is more uniformly dispersed in the fabric 2, the antibacterial property of the fabric 2 can be enhanced, and the breaking strength of the fiber is improved; the fiber has good flame retardance;
s2: compounding an azo modified graphene material and a titanium dioxide photocatalytic nano-structure material according to a ratio of 1-2; distilled water was added to the compounded finish, and the finish and distilled water were diluted in a ratio of 1.
S3: the finishing agent is sprayed onto the fabric 2 by a vacuum atomization negative pressure adsorption method.
The nano titanium dioxide decomposes bacteria under the photocatalysis to achieve the antibacterial effect. Because the electronic structure of the nano titanium dioxide is characterized by a full TiO2 valence band and an empty conduction band, in a system of water and air, when the electron energy reaches or exceeds the band gap energy of the nano titanium dioxide under the irradiation of sunlight, particularly ultraviolet rays, electrons can be excited from the valence band to the conduction band, corresponding holes are generated in the valence band, namely, electrons are generated, and the holes are separated from the electrons under the action of an electric field and migrate to different positions on the surface of particles to generate a series of reactions.
TiO2 + hν e —— + h
H2O + h—— ·OH+ H
O2 +e—— O2 ·
O2 ·+ H—— HO2·
2HO2· —— O2 + H2O2
H2O2 +O2 · —— ·OH+OH +O2
Oxygen dissolved on the surface of TiO2 is adsorbed to capture electrons to form O2. The generated superoxide anion free radical reacts (oxidizes) with most organic matters and can react with the organic matters in bacteria to generate CO2 and H2O; the cavity oxidizes OH and H2O adsorbed on the surface of TiO2 into OH which has strong oxidizing power, attacks unsaturated bonds of organic matters or extracts H atoms to generate new free radicals to excite chain reaction, and finally causes bacteria to decompose.
The TiO2 with the nanometer dispersion degree is only required to be subjected to nanosecond, picosecond and even femtosecond time for transferring the light-excited electrons and holes from the inside of the body to the surface. The composition of the photo-generated electrons and the holes is in nanosecond level, and the photo-generated electrons and the holes can be quickly transferred to the surface to attack bacterial organisms, so that the corresponding antibacterial effect is achieved.
Further, the vacuum atomization negative pressure adsorption method comprises the following specific implementation steps:
s3.1, conveying the fabric 2 by adopting a negative pressure roller in a vacuum spraying chamber; the upper surface and the lower surface of the fabric 2 are both provided with spray nozzles 101, in order to improve the spray effect, the spray height can be adjusted, the spray receiving area of the fabric 2 is changed, and the distance between the spray nozzles 101 and the surface of the fabric 2 is 1.2-1.6m;
the negative pressure in the negative pressure roller is controlled by an induced draft fan, specifically, an air inlet of the induced draft fan is formed in the surface of the negative pressure roller, the air inlet is attached to the fabric 2, and the finishing agent sprayed by the spray nozzle 101 is introduced to the surface of the fabric 2 through the negative pressure roller;
s3.2, in the process of conveying the fabric 2 through the negative pressure roller, the surface of the fabric 2 is atomized and sprayed in a multi-surface spraying mode at the flow rate of 12-15mL/min under the air pressure of 0.5-0.7Mpa, so that the surface tension of finishing agent liquid is broken under the action of pressure to be changed into fine aerial fog with the diameter of less than 3 mu m;
s3.3, sending the sprayed fabric 2 into a drying chamber, and carrying out high-temperature shaping on the fabric 2 at 180-200 ℃ for 2-3S;
and S3.4, conveying the sprayed wet fabric 2 into a heat setting machine, after the surface of the fabric 2 is heated to the setting temperature within 2-3S, destroying weak valence cross bonds in the fiber structure after the setting temperature is reached, reorienting fiber molecular chains, and quickly cooling the fabric 2 to room temperature within 2-3S before leaving the negative pressure roller conveyor.
Placing the fabric 2 in a high-temperature environment of 180-200 ℃ under a tension state to keep the fabric 2 in a certain size, so that weak valence cross bonds in a fiber structure are destroyed, and fiber molecular chains are reoriented to finish shaping.
Specifically, the negative pressure rollers are arranged along the upper and lower surfaces of the fabric 2 in a staggered manner, and the number of the negative pressure rollers distributed up and down per meter of the fabric, and the suction force of a single negative pressure roller are configured such that the surface tension of the fabric is 85-95mN/m.
Preferably, the number of the negative pressure rollers distributed up and down per meter of fabric is 3-4, and the value of the adsorption force is 6-10Pa.
Preferably, the spray nozzles 101 are arranged above and below the fabric 2 in pairs, and one of the spray nozzles 101 is connected to a positive electrode, and the other spray nozzle 101 is connected to a negative electrode, so that the sprayed and atomized finishing agent contains charged particles.
Specifically, the voltage value between the anode and the cathode is 60-80V.
After the spray nozzle is electrified, the generated charged particles accelerate the drifting of the atomized material, the scattering of the charged particles is enhanced through mutual repulsion of the same sides of the charged particles, and the larger the scattering degree is, the higher the spray concentration is; while the charged particles on both sides attract each other to increase their precipitation attraction.
S4: and (3) feeding the fabric 2 into a drying chamber, drying the fabric 2, and setting at a high temperature of 180-200 ℃ for 2-3 s.
The finishing agent is compounded with the fabric 2 by a vacuum atomization negative pressure adsorption method, the process is relatively simple, and the finishing agent is easy to be applied to the textile fabric on a large scale.
On the other hand, the invention provides a textile prepared by the preparation method of the azo modified graphene-based antibacterial and deodorant textile, which is used for the textile 2 treated by the vacuum atomization negative pressure adsorption method, as shown in fig. 3, the textile comprises a textile layer 201, a graphene layer 202 coated on the surface of the textile layer 201, and the textile 2 sprayed by a finishing agent, and has strong antibacterial property of the azo modified graphene material and the deodorizing effect of the titanium dioxide photocatalytic nanostructure material, and meanwhile, the azo modified graphene material and the titanium dioxide photocatalytic nanostructure material cooperate with each other to realize antibacterial and deodorant effects, so that the antibacterial and deodorant performance of the textile 2 can be further enhanced; at the graphite alkene layer 202 of the formation on fabric layer 201 surface, when protecting 2 top layers of fabrics, graphite alkene layer 202 mixes titanium dioxide photocatalysis nanostructured material, can strengthen the antibiotic deodorization ability of fabric 2, makes the antibiotic deodorization effect of fabric can add lastingly.
The preparation method of the azo modified graphene-based antibacterial and deodorant textile provided by the invention is further illustrated by the following specific examples according to different raw material dosages.
Example 1
S1: preparing an azo modified graphene material;
s2: mixing an azo modified graphene material and a titanium dioxide photocatalytic nano-structure material according to the ratio of 1:1, compounding in proportion; distilled water is added into the finishing agent obtained by compounding to dilute by 2.5 times.
S3: spraying the finishing agent onto the fabric 2 by a vacuum atomization negative pressure adsorption method;
s4: and (3) feeding the fabric 2 into a drying chamber, drying the fabric 2 and shaping at high temperature.
Example 2
S1: preparing an azo modified graphene material;
s2: mixing an azo modified graphene material and a titanium dioxide photocatalytic nano-structure material according to the ratio of 2:1, compounding in proportion; distilled water is added into the finishing agent obtained by compounding to dilute the finishing agent by 2.5 times.
S3: spraying the finishing agent onto the fabric 2 by a vacuum atomization negative pressure adsorption method;
s4: and (3) feeding the fabric 2 into a drying chamber, drying the fabric 2 and shaping at high temperature.
Example 3
S1: preparing an azo modified graphene material;
s2: mixing an azo modified graphene material and a titanium dioxide photocatalytic nano-structure material according to the ratio of 1:2, compounding in proportion; distilled water is added into the finishing agent obtained by compounding to dilute the finishing agent by 2.5 times.
S3: spraying the finishing agent onto the fabric 2 by a vacuum atomization negative pressure adsorption method;
s4: and (3) feeding the fabric 2 into a drying chamber, drying the fabric 2 and shaping at high temperature.
The antibacterial and deodorant textiles prepared in example 1, example 2 and example 3 were subjected to the following procedures in GB/T20944.3 evaluation of antibacterial properties of textiles part 3: the antibacterial and deodorant performance of the textile is evaluated according to the standards of an oscillation method and GB/T33610 'determination of deodorant performance of the textile', and the results are as follows:
TABLE 1 Fabric bacteriostasis and odor concentration reduction rate under finishing agent prepared from raw materials with different mixture ratios
Figure 558529DEST_PATH_IMAGE001
As can be seen from table 1, the fabrics 2 prepared by spraying finishing agents with different proportions have good antibacterial performance and deodorization performance, the antibacterial rate is the best in the case of relatively high content of azo modified graphene material in example 2, and the deodorization performance is the best in the case of relatively high content of titanium dioxide photocatalytic nanostructure material in example 3;
therefore, on the premise of ensuring the best deodorization performance of the fabric 2, taking the example 3 as the best example, in order to verify the influence of the azo modified graphene material and the titanium dioxide photocatalytic nanostructure material on the fabric 2 in the textile prepared in the example 3 of the present invention, the following comparative examples are used to comparatively illustrate the preparation method of the azo modified graphene-based antibacterial deodorization textile provided in the example of the present invention.
Comparative example 1
The comparative example adopts the preparation method of the example 3 to remove the titanium dioxide photocatalysis nano-structure material, and the other raw materials and the method are unchanged, and the specific steps are as follows:
s1: preparing an azo modified graphene material;
s2: adding distilled water into the azo modified graphene material to dilute the azo modified graphene material by 2.5 times;
s3: spraying the finishing agent onto the fabric 2 by a vacuum atomization negative pressure adsorption method;
s4: and (3) feeding the fabric 2 into a drying chamber, drying the fabric 2 and shaping at a high temperature.
Comparative example 2
The comparative example adopts the preparation method of example 3 to remove the azo-modified graphene material, and the remaining raw materials and method are unchanged, and the specific steps are as follows:
s1: adding distilled water into the titanium dioxide photocatalysis nano-structure material for diluting by 2.5 times;
s2: spraying the finishing agent onto the fabric 2 by a vacuum atomization negative pressure adsorption method;
s3: and (3) feeding the fabric 2 into a drying chamber, drying the fabric 2 and shaping at high temperature.
The antibacterial and deodorizing textiles obtained in comparative examples 1 and 2 were subjected to antibacterial and odor-reducing tests, and the results of comparison with example 3 are shown in table 2:
TABLE 2 bacteriostatic ratio of fabric and odor concentration reduction rate
Figure 865883DEST_PATH_IMAGE002
Through analysis of the table 2, the fabrics 2 prepared by spraying finishing agents with different proportions have better antibacterial performance and peculiar smell reduction performance, compared with the example 3, after the titanium dioxide photocatalysis nanostructure material is removed in the comparative example 1, the antibacterial rate is slightly reduced, but the antibacterial rate is in a normal range, and the peculiar smell reduction performance of the fabrics 2 is obviously reduced; in the comparative example 2, after the azo modified graphene material is removed, the bacteriostatic rate of the fabric 2 is obviously reduced, and the odor reduction performance is improved compared with that of the comparative example 1; it can be seen that the titanium dioxide photocatalytic nanostructure material affects the odor reduction performance of the fabric 2; the azo-modified graphene material is a conclusion that the antibacterial property of the fabric 2 is influenced.
The azo modified graphene material generates active groups, so that the antibacterial property of the fabric 2 can be enhanced, the breaking strength of the fibers is improved, meanwhile, the titanium dioxide photocatalysis nano-structure material has the deodorization effect, and the azo modified graphene material and the titanium dioxide photocatalysis nano-structure material can cooperate with each other to realize antibacterial deodorization, so that the fabric 2 has excellent antibacterial deodorization performance, the whole finishing process is environment-friendly, the effect is uniform and stable, and the antibacterial deodorization effect is lasting.
The foregoing shows and describes the general principles, essential features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, and the preferred embodiments of the present invention are described in the above embodiments and the description, and are not intended to limit the present invention. The scope of the invention is defined by the appended claims and equivalents thereof.

Claims (10)

1. An azo-modified graphene, comprising:
10-20 parts of graphene particles with the particle size of 0.1-0.2 micrometer, 6-8 parts of 2-bromoisobutyryl bromide, 15-25 parts of modified grafted polyethyl methacrylate and 1-2 parts of 4-cyanoaniline diazonium salt to perform diazo coupling reaction to obtain a graphene material with the surface grafted with azo polymer; then adding 3-5 parts of potassium phosphate and 5 parts of calcium carbonate;
mixing the above components at 60-80 deg.C in sealed environment.
2. The azo-modified graphene of claim 1, wherein the water content of the mixed composition is between 15% and 20%.
3. An antibacterial and deodorant textile is characterized in that: use of the graphene material according to any one of claims 1-2 to form a graphene layer of a fabric, the fabric (2) treated by vacuum atomization negative pressure adsorption process comprising a fabric layer (201), the graphene layer (202) coated on the surface of the fabric layer (201).
4. A preparation method of an antibacterial and deodorant textile based on azo modified graphene is characterized in that the graphene material of any one of claims 1-2 is used; the method comprises the following steps:
s1: preparing an azo modified graphene material;
s2: compounding an azo modified graphene material and a titanium dioxide photocatalytic nano-structure material to prepare a finishing agent, and adding distilled water into the finishing agent for dilution;
s3: spraying the finishing agent onto the fabric (2) by a vacuum atomization negative pressure adsorption method;
s4: and (3) feeding the fabric (2) into a drying chamber, drying the fabric (2), and setting at a high temperature of 180-200 ℃ for 2-3 s.
5. The preparation method of the azo-modified graphene-based antibacterial and deodorant textile according to claim 4, characterized by comprising the following steps: in S1, the preparation method of the azo modified graphene material comprises the following steps:
s1.1, preparing graphene oxide by a chemical method, and reducing the graphene oxide by hydrazine hydrate to obtain reduced graphene oxide;
s1.2, grafting a functional group with hydroxyl on the surface of the reduced graphene oxide through diazo addition reaction;
s1.3, reacting a functional group with hydroxyl with 2-bromine isobutyryl bromide through a Schnutten-Baumann reaction to prepare a polymerization initiator with atom transfer radical on the surface;
s1.4, initiating an atom transfer radical polymerization reaction of a monomer alkene-methyl acrylate copolymer by using an initiator, and carrying out in-situ polymerization on the surface of graphene to obtain modified grafted polyethyl methacrylate;
s1.5, carrying out diazo coupling reaction on the modified grafted polyethylmethacrylate and 4-cyanoaniline diazonium salt to obtain the graphene material with the surface grafted with the azo polymer.
6. The preparation method of the azo-modified graphene-based antibacterial and deodorant textile according to claim 4, characterized by comprising the following steps: in the S2, the azo modified graphene material and the titanium dioxide photocatalytic nano-structure material are compounded according to the proportion of 1-2; adding distilled water into the finishing agent obtained by compounding, diluting the finishing agent and the distilled water according to the ratio of 1.
7. The preparation method of the azo-modified graphene-based antibacterial and deodorant textile according to claim 4, characterized by comprising the following steps: in S3, the vacuum atomization negative pressure adsorption method comprises the following specific implementation steps:
s3.1, conveying the fabric (2) by adopting a negative pressure roller in a vacuum spraying chamber;
s3.2, in the process of conveying the fabric (2) through the negative pressure roller, the surface of the fabric (2) is atomized and sprayed in a multi-surface spraying mode at the flow rate of 12-15mL/min under the air pressure of 0.5-0.7Mpa, so that the surface tension of finishing agent liquid is broken under the action of pressure to be changed into fine aerial fog with the diameter of less than 3 um;
s3.3, conveying the sprayed fabric (2) into a drying chamber, and carrying out high-temperature setting on the fabric (2) at 180-200 ℃ for 2-3S;
and S3.4, feeding the sprayed wet fabric (2) into a heat setting machine, and quickly cooling the fabric (2) to room temperature within 2-3S before the fabric (2) leaves the negative pressure roller conveyor after the surface of the fabric (2) is heated to the setting temperature within 2-3S.
8. The preparation method of the azo modified graphene-based antibacterial and deodorant textile according to claim 4, characterized by comprising the following steps: in the S3.1, the upper surface and the lower surface of the fabric (2) are both provided with spraying nozzles (101), and the distance between the spraying nozzles (101) and the surface of the fabric (2) is 1.2-1.6m; negative pressure is controlled by the induced draft fan in the negative pressure cylinder, sets up the air intake of induced draft fan on the negative pressure cylinder surface, and the air intake is laminated with fabric (2), will spray the finishing agent that mouth (101) sprayed and lead to fabric (2) surface through the negative pressure cylinder.
9. The preparation method of the azo-modified graphene-based antibacterial and deodorant textile according to claim 8, characterized in that: in the S3.4, the fabric (2) is placed in a high-temperature environment of 180-200 ℃ in a tension state; the negative pressure rollers are arranged along the upper surface and the lower surface of the fabric (2) in a staggered mode, the number of the negative pressure rollers distributed up and down per meter of the fabric and the adsorption force of each negative pressure roller are configured to enable the surface tension of the fabric to be 85-95mN/m; the number of the negative pressure rollers distributed up and down per meter of fabric is 3-4, and the value of the adsorption force is 6-10Pa.
10. The preparation method of the azo modified graphene-based antibacterial and deodorant textile according to claim 9, characterized by comprising the following steps: the spray nozzles (101) are arranged above and below the fabric (2) in pairs, one spray nozzle (101) is connected with the positive electrode, and the other spray nozzle (101) is connected with the negative electrode, so that the sprayed and atomized finishing agent contains charged particles.
CN202310024690.3A 2023-01-09 2023-01-09 Azo modified graphene, antibacterial and deodorant textile and preparation method thereof Pending CN115976829A (en)

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