CN114622295A - Antibacterial regenerated cellulose material and preparation method thereof - Google Patents
Antibacterial regenerated cellulose material and preparation method thereof Download PDFInfo
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- CN114622295A CN114622295A CN202210139102.6A CN202210139102A CN114622295A CN 114622295 A CN114622295 A CN 114622295A CN 202210139102 A CN202210139102 A CN 202210139102A CN 114622295 A CN114622295 A CN 114622295A
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F2/00—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof
- D01F2/06—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof from viscose
- D01F2/08—Composition of the spinning solution or the bath
Abstract
The invention discloses an antibacterial regenerated cellulose material which is prepared from spinning solution through a spinning process, wherein the spinning solution comprises the following components: MoS2Nanoparticle, acrylonitrile and viscose spinning dope, wherein the MoS2The nano particles account for 0.01-0.1% of the total mass of the spinning solution, the acrylonitrile accounts for 2-10% of the total mass of the spinning solution, and the viscose spinning dope accounts for 90-96% of the total mass of the spinning solution. The invention also discloses a preparation method of the antibacterial regenerated cellulose material and a regenerated cellulose fabric prepared from the antibacterial regenerated cellulose material. The regenerated cellulose material has excellent and durable antibacterial function, and the strength of the regenerated cellulose material is greatly improved compared with that of common viscose fibers.
Description
Technical Field
The invention relates to the technical field of cellulose materials, in particular to an antibacterial regenerated cellulose material and a preparation method thereof.
Background
Textile material refers to fibers and fibrous articles, embodied as fibers, yarns, fabrics, and composites thereof. Conventional textile materials are primarily referred to as fibers, which are the basic unit of the textile material. The fibers are divided into two main categories, natural fibers and chemical fibers. Natural fibers are classified into plant-based fibers, animal-based fibers and mineral-based fibers according to the material origin properties of the fibers. According to the difference of raw materials, processing methods and components, the fiber can be divided into three types of regenerated fiber, synthetic fiber and inorganic fiber. The traditional textile industry processes natural or man-made fibres or reprocesses them with ready-made textile materials to obtain the raw materials from which the relevant articles are made. With the improvement of living standard, people have higher and higher requirements on textile materials, which not only have high requirements on beauty, but also have higher expectations on safety, environmental protection and comfort, and the textile materials are required to have additional performances such as ultraviolet resistance, antibiosis and the like besides basic fabric performances. The antibacterial textile material is a fiber or fabric which has the effect of killing or inhibiting microorganisms such as bacteria, fungi, viruses and the like, and the purpose of the antibacterial textile material is not only to prevent the textile from being polluted and damaged by the microorganisms, but also more importantly to prevent infectious diseases, ensure the health and the wearing comfort of human bodies, reduce the cross infection rate of public environments and enable the textile to obtain a new health-care function.
The chemical composition and performance of the regenerated cellulose are similar to those of cotton fiber, the moisture absorption is higher than that of the cotton fiber, the regenerated cellulose has better hand feeling, but both the cellulose fiber and the regenerated cellulose fiber have no antibacterial performance, and the strength is lower than that of the cotton fiber.
At present, the antibacterial performance of the fabric is improved, and an antibacterial finishing agent is generally adopted. Chinese patents such as CN105350293B, CN 102877287B, CN104278527B and CN104264482B all disclose that antibacterial finishing liquor is used to perform antibacterial finishing on fabrics to impart antibacterial performance to the fabrics. However, these conventional antibacterial finishing agents generally adopt esters or hydroxyl groups to bond with hydrogen bonds in hydroxyl groups on the fabric, and although the overall fastness is good, after 10 times of washing, the antibacterial performance is greatly reduced, and the antibacterial performance is lost over time.
Disclosure of Invention
The technical problem to be solved by the invention is to provide an antibacterial regenerated cellulose material which has an excellent and durable antibacterial function and the strength of which is greatly improved compared with that of common viscose fibers.
In order to solve the technical problems, the invention provides the following technical scheme:
the invention provides an antibacterial regenerated cellulose material, which is prepared from a spinning solution through a spinning process, wherein the spinning solution comprises the following components: MoS2Nanoparticle, acrylonitrile and viscose spinning dope, wherein the MoS2The nano particles account for 0.01-0.1% of the total mass of the spinning solution, the acrylonitrile accounts for 2-10% of the total mass of the spinning solution, and the viscose spinning dope accounts for 90-96% of the total mass of the spinning solution.
MoS2Is a photocatalytic material, and under the condition of light, MoS2Active oxygen sterilization is generated, thereby killing bacteria and microorganisms on the surface of the fabric. The nano particles have large specific surface area and high activity, can reach the reaction speed which is more than 10 times of that of a common catalyst in the catalytic process, and MoS can be obtained under photocatalysis2The speed and the quantity of OH free radicals generated and adsorbed on the surfaces of the nano particles are greatly increased, so that the MoS is effectively improved2The bacteriostatic effect of the composition. In the invention, 0.01-0.1% of MoS is added into viscose spinning solution2Nanoparticles, after spinning, MoS2The nano particles are uniformly distributed in the interior and on the surface of the fiber, so that the excellent antibacterial effect is achieved, the antibacterial effect is stable and long-lasting, and after multiple times of washing, the antibacterial activity is slightly reduced, which is far superior to that of the existing fiber fabric treated by the antibacterial finishing agent. Preferably, the MoS2The addition amount of the nano particles accounts for 0.02 to 0.08 percent of the total mass of the spinning solution, and is more preferably 0.05 percent.
In the present invention, the MoS2The particle size of the nanoparticles is preferably in the range of 3 to 10nm, and may be, for example, 4nm, 5nm, 6nm, 7nm, 8nm, 9nm, or the like. The inventor finds that MoS through experiments2The particle size of the nanoparticles has a great influence on the bacteriostatic properties. When MoS2When the particle size of the antibacterial agent is less than 10nm, the antibacterial effect can be greatly improved under the condition of solar illumination; but when the particle size is more than 10nm, the bacteriostatic effect is greatly reduced. Therefore, when MoS2When the particle size distribution range of the nano particles is 3-10 nm, the prepared antibodyThe bacteria regenerated cellulose material has better bacteriostatic effect.
In addition, the strength of the regenerated cellulose fiber is lower than that of cotton fiber, in order to improve the strength, 2-10% of acrylonitrile is added into viscose spinning solution, acrylonitrile molecules have active groups such as C-C double bonds and C-N triple bonds, and the addition of the acrylonitrile increases chemically active groups in the viscose spinning solution and can generate double bond addition reaction with groups such as-OH, hydrogen bonds and the like existing on the cellulose molecules, so that the crosslinking of the cellulose molecules is realized, and the strength of the regenerated cellulose material is greatly improved due to the increase of the polymerization degree. Preferably, the addition amount of acrylonitrile is 4% to 9%, more preferably 9%, of the total mass of the spinning solution.
In the present invention, the viscose spinning solution is commercially available from various large chemical fiber factories, and is a raw material for producing regenerated cellulose fibers (viscose fibers) in the chemical fiber factories, and the main component is cellulose.
The invention also provides a preparation method of the antibacterial regenerated cellulose material, which comprises the following steps:
s1, mixing acrylonitrile and MoS2Mixing the nano particles, and stirring uniformly to obtain a uniform solution;
s2, adding the solution into viscose spinning solution according to a proportion, uniformly stirring to obtain spinning solution, and spinning the spinning solution to obtain the antibacterial regenerated cellulose material.
Further, in step S1, the temperature of the system is controlled to be 60 to 65 ℃ during stirring.
Further, in step S1, the rotation speed during stirring is 400 to 450 rpm.
Further, in step S2, the rotation speed during stirring is 100 to 150 rpm.
The invention also provides an antibacterial regenerated cellulose fabric which is prepared from the antibacterial regenerated cellulose material through a weaving process.
Further, the gram weight of the antibacterial regenerated cellulose fabric is 120-123 g/m2Breaking strength of over 300N, against Staphylococcus aureus and large intestineThe bacteriostatic rate of bacillus is over 95 percent.
Compared with the prior art, the invention has the beneficial effects that:
1. the invention adds acrylonitrile and molybdenum disulfide nano particles (MoS) in the preparation process of the regenerated cellulose material2) The characteristic that molybdenum disulfide nano particles generate active oxygen under photocatalysis is utilized to endow the fiber with good antibacterial performance, and simultaneously MoS is utilized2The nano particles are uniformly distributed in the fiber and on the surface of the fiber, so that the excellent antibacterial effect is achieved, the antibacterial effect is stable and long-lasting, and the antibacterial activity is slightly reduced after the fiber is washed for many times; in addition, the double bond addition reaction between acrylonitrile and cellulose is utilized to realize the crosslinking of the regenerated cellulose, so that the strength of the regenerated cellulose material is greatly improved.
2. The preparation process of the regenerated cellulose fabric prepared by the invention is simple and convenient, the acrylonitrile and the molybdenum disulfide nano particles are added into the spinning solution according to the proportion, and the viscose fabric can be obtained through spinning and a manufacturing process; in addition, the processed viscose fabric has excellent antibacterial performance, the fabric strength can be improved by more than 20%, and the use performance of the fabric is greatly improved.
Drawings
Fig. 1 is a diagram of the bacteriostatic effect of the bacteriostatic high-strength viscose fabric of example 1 on staphylococcus aureus (a) and escherichia coli (b).
Detailed Description
The present invention is further described below in conjunction with the following figures and specific examples so that those skilled in the art may better understand the present invention and practice it, but the examples are not intended to limit the present invention.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
The experimental methods used in the following examples are conventional methods unless otherwise specified, and materials, reagents and the like used therein are commercially available without otherwise specified.
In the following examples and comparative examples, viscose spinning solutions used were purchased from Xinxiang chemical fiber Co., Ltd, and cellulose was used as a main component; MoS of various particle sizes2The nanoparticles were purchased from Nanjing Xiancheng nanomaterial science and technology Co.
1. The preparation method of the spinning solution comprises the following steps:
the first step is as follows: firstly, adding acrylonitrile into a stirring container, controlling the temperature to be 60-65 ℃, and gradually adding MoS2Stirring uniformly at a stirring speed of 400-450 rpm to obtain a uniform solution.
The second step is that: and slowly adding the solution into the viscose spinning solution according to a proportion, uniformly stirring, and spinning when the stirring speed is 100-150 rpm.
2. The weaving method of the bacteriostatic high-strength viscose fabric in the examples and the comparative examples comprises the following steps:
opening picking (the beating speed is 400-.
3. Common viscose (without acrylonitrile and MoS addition)2) The weaving method comprises the following steps:
opening picking (the beating speed is 350-.
Example 1
In this example, the raw materials were: MoS2(the particle size range is 5-8 nm, the mass of the acrylonitrile accounts for 0.072% of the mass of the spinning solution), and the acrylonitrile accounts for 8% of the mass of the spinning solutionAnd viscose dope (91.928% of dope quality).
MoS was treated as described above2The acrylonitrile and the viscose spinning solution are prepared into spinning solution and are woven into bacteriostatic high-strength viscose fabric with the gram weight of 121.7g/m2。
The rupture strength and the bacteriostatic performance of the prepared bacteriostatic high-strength viscose fabric are tested, and the results are shown in table 1 and attached figure 1. The standard of the test is as follows:
antibacterial property (bacteriostatic ratio): GB 20944.3-2008-T evaluation of antibacterial properties of textiles part 3: and (4) testing by an oscillation method. Breaking strength: according to GB/T3923.1-2013 part 1 of tensile properties of textile fabrics: determination of breaking strength and breaking elongation (bar method).
Table 1 example 1 performance test of bacteriostatic high-strength viscose fabric
Note: "-" indicates that the bacteriostatic performance is lower than 75%, indicating no bacteriostatic effect.
As can be seen from the results in table 1, the breaking strength of the viscose fabric prepared in this example is significantly higher than that of the common viscose fabric; in addition, the viscose fabric also has antibacterial performance, has good inhibition effect on staphylococcus aureus and escherichia coli, and after being washed for 20 times, the antibacterial performance is only slightly reduced, so that good antibacterial stability is shown.
The results in fig. 1 further demonstrate that the viscose fabric prepared in this example has good inhibitory effect on staphylococcus aureus and escherichia coli.
Example 2
In this example, the raw materials were: MoS2(the particle size is 5-8 nm and accounts for 0.05% of the mass of the spinning solution), acrylonitrile (accounts for 6% of the mass of the spinning solution) and viscose spinning solution (accounts for 93.95% of the mass of the spinning solution).
MoS was treated as described above2Acrylonitrile and viscose spinning solution are prepared into spinning solution,and weaving into bacteriostatic high-strength viscose fabric with the gram weight of 121.4g/m2。
The rupture strength and the bacteriostatic performance of the prepared bacteriostatic high-strength viscose fabric are tested, and the results are shown in table 2.
Table 2 example 2 performance test of bacteriostatic high-strength viscose fabric
Example 3
In this example, the raw materials were: MoS2(the particle size is 5-8 nm and accounts for 0.025% of the mass of the spinning solution), acrylonitrile (accounts for 4% of the mass of the spinning solution) and viscose spinning solution (accounts for 95.975% of the mass of the spinning solution).
MoS was treated as described above2Acrylonitrile and viscose spinning solution are prepared into spinning solution and are woven into bacteriostatic high-strength viscose fabric with the gram weight of 121.9g/m2。
The rupture strength and the bacteriostatic performance of the prepared bacteriostatic high-strength viscose fabric are tested, and the results are shown in table 3.
Table 3 example 3 performance test of bacteriostatic high-strength viscose fabric
Example 4
In this example, the raw materials were: MoS2(the particle size is 5-8 nm and accounts for 0.04% of the mass of the spinning solution), acrylonitrile (accounts for 4% of the mass of the spinning solution) and viscose spinning solution (accounts for 95.96% of the mass of the spinning solution).
MoS was treated as described above2The acrylonitrile and the viscose spinning solution are prepared into spinning solution and woven into bacteriostatic high-strength viscose fabric with the gram weight of 120.8g/m2。
The rupture strength and the bacteriostatic performance of the prepared bacteriostatic high-strength viscose fabric are tested, and the results are shown in table 4.
Table 4 example 4 performance test of bacteriostatic high-strength viscose fabric
Example 5
In this example, the raw materials were: MoS2(the particle size is 5-8 nm and accounts for 0.072% of the mass of the spinning solution), acrylonitrile (accounts for 4% of the mass of the spinning solution) and viscose spinning solution (accounts for 95.928% of the mass of the spinning solution).
MoS was treated as described above2The acrylonitrile and the viscose spinning solution are prepared into spinning solution and woven into bacteriostatic high-strength viscose fabric with the gram weight of 122.9g/m2。
The rupture strength and the bacteriostatic performance of the prepared bacteriostatic high-strength viscose fabric are tested, and the results are shown in table 5.
Table 5 example 5 performance test of bacteriostatic high-strength viscose fabric
Example 6
In this example, the raw materials were: MoS2(the particle size is 5-8 nm and accounts for 0.025% of the mass of the spinning solution), acrylonitrile (accounts for 9% of the mass of the spinning solution) and viscose spinning solution (accounts for 90.975% of the mass of the spinning solution).
MoS was treated as described above2The acrylonitrile and the viscose spinning solution are prepared into spinning solution and are woven into bacteriostatic high-strength viscose fabric with the gram weight of 121.7g/m2。
The rupture strength and the bacteriostatic performance of the prepared bacteriostatic high-strength viscose fabric are tested, and the results are shown in table 6.
Table 6 example 6 performance test of bacteriostatic high-strength viscose fabric
Comparative example 1
In this comparative example, the raw materials were as follows: MoS2(the particle size is 10-15 nm and accounts for 0.072% of the mass of the spinning solution), acrylonitrile (accounting for 9% of the mass of the spinning solution) and viscose spinning solution (accounting for 90.928% of the mass of the spinning solution).
MoS was treated as described above2And the acrylonitrile and the viscose spinning solution are prepared into spinning solution and woven into the antibacterial high-strength viscose fabric.
The rupture strength and the bacteriostatic performance of the prepared bacteriostatic high-strength viscose fabric are tested, and the results are shown in table 7.
TABLE 7 Performance test of antibacterial high-strength viscose fabric in comparative example 1
Comparative example 2
In this comparative example, the raw materials were as follows: MoS2(the particle size range is 12-15 nm and accounts for 0.072% of the mass of the spinning solution), and viscose spinning solution (accounts for 99.928% of the mass of the spinning solution).
MoS was treated as described above2And preparing the spinning solution with viscose spinning solution, and weaving the spinning solution into the antibacterial viscose fabric.
The prepared antibacterial viscose fabric is tested for breaking strength and antibacterial performance, and the results are shown in table 8.
Table 8 performance test of antibacterial viscose fabric in comparative example 2
Comparative example 3
In this comparative example, the raw materials were as follows: MoS2(the particle size is 5-8 nm and accounts for 0.072% of the mass of the spinning solution), and viscose spinning solution (accounts for99.928% of the mass of the spinning dope).
MoS was treated as described above2And preparing the spinning solution with viscose spinning solution, and weaving the spinning solution into the antibacterial viscose fabric.
The prepared antibacterial viscose fabric is tested for breaking strength and antibacterial performance, and the results are shown in table 9.
TABLE 9 Performance testing of the bacteriostatic viscose fabric of comparative example 3
Comparative example 4
In this comparative example, the raw materials were as follows: MoS2(the particle size is 5-8 nm and accounts for 0.025 percent of the mass of the spinning solution), and viscose spinning solution (accounts for 99.975 percent of the mass of the spinning solution).
MoS was treated as described above2Preparing the mixture into spinning solution with viscose spinning solution, and weaving the spinning solution into antibacterial viscose fabric (the gram weight is 120.9 g/m)2)。
The prepared antibacterial viscose fabric is tested for breaking strength and antibacterial performance, and the results are shown in table 10.
TABLE 10 Performance testing of the bacteriostatic viscose fabric of comparative example 4
Comparative example 5
In this comparative example, the raw materials were as follows: acrylonitrile (accounting for 9% of the mass of the spinning solution) and viscose spinning solution (accounting for 91% of the mass of the spinning solution).
According to the method, the acrylonitrile and the viscose spinning solution are prepared into spinning solution, and the spinning solution is woven into the high-strength viscose fabric.
The prepared high-strength viscose fabric was tested for breaking strength and bacteriostatic properties, and the results are shown in table 11.
TABLE 11 Performance testing of high strength viscose fabrics of comparative example 5
Comparative example 6
In this comparative example, the raw materials were as follows: acrylonitrile (accounting for 4% of the mass of the spinning solution) and viscose spinning solution (accounting for 96% of the mass of the spinning solution).
According to the method, the acrylonitrile and the viscose spinning solution are prepared into spinning solution, and the high-strength viscose fabric is woven.
The prepared high-strength viscose fabric was tested for breaking strength and bacteriostatic properties, and the results are shown in table 12.
TABLE 12 Performance testing of high tenacity viscose fabric of comparative example 6
Comparative example 7
In this comparative example, the raw materials were as follows: acrylonitrile (accounting for 3% of the mass of the spinning solution) and viscose spinning solution (accounting for 97% of the mass of the spinning solution).
According to the method, the acrylonitrile and the viscose spinning solution are prepared into spinning solution, and the high-strength viscose fabric is woven.
The prepared high-strength viscose fabric was tested for breaking strength and antibacterial performance, and the results are shown in table 13.
TABLE 13 Performance testing of high tenacity viscose fabric of comparative example 7
Comparative example 8
In this comparative example, the raw materials were as follows: acrylonitrile (accounting for 1 percent of the mass of the spinning solution) and viscose spinning solution (accounting for 99 percent of the mass of the spinning solution).
According to the method, the acrylonitrile and the viscose spinning solution are prepared into spinning solution, and the high-strength viscose fabric is woven.
The prepared high-strength viscose fabric was tested for breaking strength and bacteriostatic properties, and the results are shown in table 14.
TABLE 14 Performance testing of high tenacity viscose fabric of comparative example 8
As is clear from the results of examples 1 to 6 and comparative examples 1 to 8, when MoS having a particle diameter exceeding 10nm is used2When the particle size is nanometer, the bacteriostatic property of the fabric is reduced, and the more the bacteriostatic property is reduced along with the increase of the particle size. In addition, within a certain range, the breaking strength of the fabric is increased with the increase of the addition amount of acrylonitrile.
In conclusion, the viscose spinning solution is added with a certain amount of MoS2The nano particles and the acrylonitrile, and the finally prepared regenerated cellulose fabric not only has excellent and lasting antibacterial performance, but also can improve the fabric strength by more than 20 percent, thereby greatly improving the service performance of the fabric.
The above-mentioned embodiments are merely preferred embodiments for fully illustrating the present invention, and the scope of the present invention is not limited thereto. The equivalent substitution or change made by the technical personnel in the technical field on the basis of the invention is all within the protection scope of the invention. The protection scope of the invention is subject to the claims.
Claims (10)
1. Antibacterial regenerated cellulose materialThe antibacterial regenerated cellulose material is characterized by being prepared from spinning solution through a spinning process, wherein the spinning solution comprises the following components: MoS2Nanoparticle, acrylonitrile and viscose spinning dope, wherein the MoS2The nano particles account for 0.01-0.1% of the total mass of the spinning solution, the acrylonitrile accounts for 2-10% of the total mass of the spinning solution, and the viscose spinning solution accounts for 90-96% of the total mass of the spinning solution.
2. The antimicrobial regenerated cellulose material of claim 1, wherein the MoS is2The nano particles account for 0.02-0.08% of the total mass of the spinning solution, and the acrylonitrile accounts for 4-9% of the total mass of the spinning solution.
3. The antimicrobial regenerated cellulose material of claim 1, wherein the MoS is2The particle size distribution range of the nanoparticles is 3-10 nm.
4. The antibacterial regenerated cellulose material as claimed in claim 1, wherein the viscose spinning dope is cellulose as a main component.
5. The method for preparing an antibacterial regenerated cellulose material according to any one of claims 1 to 4, characterized by comprising the steps of:
s1, mixing acrylonitrile and MoS2Mixing the nano particles, and stirring uniformly to obtain a uniform solution;
s2, adding the solution into viscose spinning solution according to a proportion, uniformly stirring to obtain spinning solution, and spinning the spinning solution to obtain the antibacterial regenerated cellulose material.
6. The method of claim 5, wherein in step S1, the temperature of the system is controlled to be 60-65 ℃ during stirring.
7. The method of claim 5, wherein the rotation speed during the stirring step S1 is 400-450 rpm.
8. The method of claim 5, wherein the rotation speed of the stirring step S2 is 100-150 rpm.
9. An antibacterial regenerated cellulose fabric, which is characterized in that the antibacterial regenerated cellulose fabric is prepared from the antibacterial regenerated cellulose material of any one of claims 1 to 4 through a weaving process.
10. The antibacterial regenerated cellulose fabric according to claim 9, characterized in that the gram weight of the antibacterial regenerated cellulose fabric is 120-123 g/m2The breaking strength is over 300N, and the bacteriostasis rate to staphylococcus aureus and escherichia coli is over 95 percent.
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