CN108978038B - Preparation method of novel non-woven fabric with antibacterial effect - Google Patents
Preparation method of novel non-woven fabric with antibacterial effect Download PDFInfo
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- CN108978038B CN108978038B CN201810928653.4A CN201810928653A CN108978038B CN 108978038 B CN108978038 B CN 108978038B CN 201810928653 A CN201810928653 A CN 201810928653A CN 108978038 B CN108978038 B CN 108978038B
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- titanium dioxide
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- woven fabric
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- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
- D04H1/42—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
- D04H1/4382—Stretched reticular film fibres; Composite fibres; Mixed fibres; Ultrafine fibres; Fibres for artificial leather
-
- 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
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
- D01F1/103—Agents inhibiting growth of microorganisms
-
- 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
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
- D01F8/06—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyolefin as constituent
-
- 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
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
- D01F8/14—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyester as constituent
Abstract
The invention relates to a preparation method of a novel non-woven fabric with an antibacterial effect, which comprises the following steps: (1) preparing modified nano titanium dioxide; (2) spinning; (3) opening; (4) carding; (5) laying a net; the novel non-woven fabric has the advantages of good antibacterial effect, high strength, no pilling in the use process and good use performance.
Description
Technical Field
The application belongs to the field of new materials, and particularly relates to a preparation method of a novel non-woven fabric with a bacteriostatic action.
Background
Nonwoven fabrics are constructed from oriented or random fibers. It is called a cloth because of its appearance and certain properties. The non-woven fabric has the characteristics of moisture resistance, air permeability, flexibility, light weight, no combustion supporting, easy decomposition, no toxicity or irritation, rich color, low price, recycling and the like. For example, the polypropylene (pp material) granules are mostly adopted as raw materials and are produced by a continuous one-step method of high-temperature melting, spinning, laying a line and hot-pressing coiling.
At present, the application range of non-woven fabrics is wider, and in some special fields, the non-woven fabrics is required to have good bacteriostatic action, often realizes through the mode of adding silver ion or other bacteriostatic agent, but, inevitably can cause the bacteriostatic agent to separate out in the use, causes the potential safety hazard.
Disclosure of Invention
The invention aims to provide a preparation method of a novel non-woven fabric with an antibacterial effect, and the antibacterial effect and safety of the non-woven fabric are obviously improved through the improvement of a process.
The invention is realized by the following technical scheme:
a preparation method of novel non-woven fabric with bacteriostatic action comprises the following steps:
(1) preparing modified nano titanium dioxide;
a. soaking nano titanium dioxide in 2mol/L sodium hydroxide solution, continuously stirring in the soaking process, and then washing with deionized water to be neutral;
b. soaking the washed nano titanium dioxide in 2mol/L acetic acid solution, carrying out ultrasonic oscillation treatment for 15-20min in the soaking process, drying at 50 ℃, mixing a silane coupling agent accounting for 0.5 percent of the weight of the nano titanium dioxide with the nano titanium dioxide, and grinding to fully and uniformly mix the nano titanium dioxide; the polarity and the adsorption performance of the surface of the nano titanium dioxide can be improved by using an acetic acid solution for treatment, and the bonding strength and the bonding stability are improved by using the reaction with a coupling agent and subsequent chitosan.
c. Adding 5 times of water by weight of chitosan into the chitosan, dropwise adding glacial acetic acid into the water to adjust the pH value to 3-4, stirring to dissolve the chitosan, mixing the nano titanium dioxide prepared in the step b and the chitosan solution according to the weight ratio of 1:4, carrying out ultrasonic oscillation treatment for 15min, carrying out vacuum filtration, and drying to obtain modified nano titanium dioxide; due to the surface modification of the nano titanium dioxide, the compatibility of the polypropylene and the polyethylene glycol terephthalate is also well promoted.
(2) Spinning;
taking 100 parts by weight of polypropylene and 40 parts by weight of polyethylene glycol terephthalate, drying, adding 1-3 parts by weight of the modified nano titanium dioxide prepared in the step (1), mixing materials by using a double-screw extruder, and then spinning;
(3) opening;
opening and mixing the spinning in the step (2) by using an opener;
(4) carding;
carding the opened spinning;
(5) laying a net;
and (3) lapping the carded spinning by using a lapping machine, finishing and forming, carrying out spun-bonding by using a double-roller hot rolling machine, and cooling and rolling.
The roll shaft temperature of the twin-roll hot rolling mill was 145 ℃.
After the spinning in the step (2), adding 10 parts of the spun yarn into 100 parts of 1.2mol/L acetic acid solution, soaking at a constant temperature of 25 ℃ for 20min, introducing nitrogen to discharge oxygen in the system, adding 10 parts of ethyl acrylate ethanol solution with the mass fraction of 5%, uniformly stirring, slowly adding 0.015 part of potassium persulfate, stirring at a speed of 500r/min in the adding process, heating to 65 ℃, continuously stirring, reacting for 50min, cooling to the normal temperature, adding 2mol/L sodium hydroxide solution to adjust the pH of the solution to 8.5, filtering the spun yarn, washing to be neutral, and drying to obtain the modified spun yarn.
In step (5), the laid mesh is treated at 60 ℃ for 60min and then treated with a twin roll hot mill.
The roller surface of two roller hot rolling mills has needle-like burr, and burr length is 0.1mm, can promote the radiating effect on roller surface for when the roll-in, ambient temperature is unanimous relatively, promotes the homogeneity of non-woven fabrics, and the burr can have acupuncture's effect to the non-woven fabrics in addition, can form the tie point that intensity is higher on the surface during the roll-in, promotes the intensity of non-woven fabrics, can further promote the joint strength of non-woven fabrics.
Preferably, the burr diameter is no greater than 0.3 mm.
The invention has the beneficial effects that: the novel non-woven fabric provided by the application utilizes the modified nano titanium dioxide as the antibacterial agent, when the novel non-woven fabric is treated, chitosan is grafted on the surface of the nano titanium dioxide, the chitosan and the titanium dioxide directly pass through the connection effect of hydrogen bonds and a coupling agent, the connection strength is better, the bacteriostatic and bactericidal effects can be obviously improved, meanwhile, when the novel non-woven fabric is spun, the nano titanium dioxide has a large specific surface area, the combination effect with polypropylene and polyethylene glycol terephthalate can be obviously improved, the spinning strength is improved, and further the strength of the non-woven fabric is obviously improved; in the application, after spinning, modification treatment is carried out on the spinning, crosslinking is generated between the spinning by utilizing the micro polymerization effect of ethyl acrylate, chitosan on the surface of the spinning and the like under the action of a catalyst, the strength of a crosslinking node is obviously improved, and although the partially crosslinked fibers are separated in subsequent treatment, the strength of materials at the crosslinking point is improved, and the strength of the non-woven fabric is also improved.
The novel non-woven fabric has the advantages of good antibacterial effect, high strength, no pilling in the use process and good use performance, and the polypropylene and the polyethylene terephthalate are compounded for wire drawing through the modification of the titanium dioxide and the adjustment of the preparation process, so that the obvious synergistic effect is achieved, and the comprehensive performance of the non-woven fabric is improved.
Detailed Description
Example 1
A preparation method of novel non-woven fabric with bacteriostatic action comprises the following steps:
(1) preparing modified nano titanium dioxide;
a. soaking nano titanium dioxide in 2mol/L sodium hydroxide solution, continuously stirring in the soaking process, and then washing with deionized water to be neutral;
b. soaking the washed nano titanium dioxide in 2mol/L acetic acid solution, carrying out ultrasonic oscillation treatment for 15-20min in the soaking process, drying at 50 ℃, mixing a silane coupling agent accounting for 0.5 percent of the weight of the nano titanium dioxide with the nano titanium dioxide, and grinding to fully and uniformly mix the nano titanium dioxide;
c. adding 5 times of water by weight of chitosan into the chitosan, dropwise adding glacial acetic acid into the water to adjust the pH value to 3-4, stirring to dissolve the chitosan, mixing the nano titanium dioxide prepared in the step b and the chitosan solution according to the weight ratio of 1:4, carrying out ultrasonic oscillation treatment for 15min, carrying out vacuum filtration, and drying to obtain modified nano titanium dioxide;
(2) spinning;
taking 100 parts by weight of polypropylene and 40 parts by weight of polyethylene glycol terephthalate, drying, adding 2.2 parts by weight of the modified nano titanium dioxide prepared in the step (1), mixing materials by using a double-screw extruder, and then spinning, wherein the spinning diameter is 10 microns;
(3) opening;
opening and mixing the spinning in the step (2) by using an opener;
(4) carding;
carding the opened spinning;
(5) laying a net;
and (3) lapping the carded spinning by using a lapping machine, finishing and forming, carrying out spun-bonding by using a double-roller hot rolling machine, and cooling and rolling.
The roll shaft temperature of the twin-roll hot rolling mill was 145 ℃.
After the spinning in the step (2), adding 10 parts of the spun yarn into 100 parts of 1.2mol/L acetic acid solution, soaking at a constant temperature of 25 ℃ for 20min, introducing nitrogen to discharge oxygen in the system, adding 10 parts of ethyl acrylate ethanol solution with the mass fraction of 5%, uniformly stirring, slowly adding 0.015 part of potassium persulfate, stirring at a speed of 500r/min in the adding process, heating to 65 ℃, continuously stirring, reacting for 50min, cooling to the normal temperature, adding 2mol/L sodium hydroxide solution to adjust the pH of the solution to 8.5, filtering the spun yarn, washing to be neutral, and drying to obtain the modified spun yarn.
In step (5), the laid mesh is treated at 60 ℃ for 60min and then treated with a twin roll hot mill.
The surface of the roller of the double-roller hot rolling mill is provided with needle-shaped burrs, and the lengths of the burrs are 0.1 mm.
Example 2
In contrast to example 1, no modification treatment was performed on the spun yarn after step (2).
Example 3
In comparison with example 1, after completion of the lapping, the hot press treatment was directly performed without performing the heat-insulating treatment at 60 ℃.
Comparative example 1
The other steps are the same as example 1 without modifying the nano titanium dioxide.
Comparative example 2
The same procedure as in example 1 was repeated except that the amount of polypropylene was adjusted to 140 parts without adding polyethylene terephthalate during spinning.
Comparative example 3
The procedure of example 1 was otherwise the same as that of example 1 except that the amount of polyethylene terephthalate was adjusted to 140 parts without adding polypropylene.
Comparative example 4
Commercially available polypropylene nonwoven fabrics.
Comparative example 5
Commercially available polyethylene terephthalate nonwoven fabrics.
Experiment 1
The nonwoven fabrics of the examples and comparative examples were verified for their performance.
The non-woven fabrics prepared by the methods of each group are subjected to performance test, the performance of the non-woven fabrics in each group is counted, and the result is shown in table 1;
table 1:
note: in the wear resistance test, 30 × 30cm of non-woven fabric is folded in half, 5kg of force is applied to the non-woven fabric to rub the folded non-woven fabric, the displacement is 5cm each time, the times when the pilling starts are the representing mode of the wear resistance, namely the times are more, the wear resistance is better.
When the antibacterial effect is tested, the concentration is 5 multiplied by 106The method comprises the following steps of uniformly smearing cfu/mL escherichia coli in a plurality of groups of culture dishes with diameters of 100mm and containing nutrient agar, cutting sample pieces with the radius of 3cm from each group of non-woven fabrics, respectively paving the sample pieces in the centers of the culture dishes, placing each group of culture dishes in a constant temperature box with the temperature of 35 ℃ for culturing for 72 hours, and measuring the number of bacterial colonies on each non-woven fabric sample piece.
When the ultraviolet resistance effect is tested, the product is placed under ultraviolet rays to irradiate for 3 hours, and the color change is observed.
As can be seen from Table 1, the material prepared in the embodiment 1 of the application has the advantages of being remarkably superior to other schemes in strength, wear resistance, antibacterial effect or ultraviolet resistance effect, and can play a role in improving the strength of the material through the modification of the nano titanium oxide in the application.
Experiment 2
In order to further verify the influence of the modification of the nano titanium oxide on the material performance, different control experiments are set,
comparative example 6
Compared with the embodiment 1, the nano titanium dioxide is not soaked by using acetic acid solution in the modification process.
Comparative example 7
Compared with the example 1, no silane coupling agent is added in the process of processing the nano titanium dioxide.
Comparative example 8
In contrast to example 1, the step c treatment was not used in the nano titania modification treatment.
The influence of different treatment modes on the performance of the nonwoven fabric is counted, and the results are shown in table 2:
table 2:
note: the titanium dioxide stability is used for representing the content of free titanium dioxide in a non-woven fabric material, the content is measured by using a metallic aluminum reduction method, before the test, 10g of non-woven fabric is soaked for 2 hours by using a 2mol/L sulfuric acid solution, then the content of the titanium dioxide in the solution is measured, the content is relatively low, the application is characterized by the relative content, "-" indicates that the free titanium dioxide is not detected, "+" indicates that the free titanium dioxide is detected, and more "+" indicates that the content of the free titanium dioxide is higher.
As can be seen from Table 2, after the nano titanium dioxide is modified by different methods, the performance of the final non-woven fabric product is affected, and after the treatment mode is changed, the strength and the wear resistance of the non-woven fabric are negatively affected, so that the treatment process of the mode in the application is proved to be better.
Claims (2)
1. A preparation method of novel non-woven fabric with bacteriostatic action is characterized by comprising the following steps:
(1) preparing modified nano titanium dioxide;
a. soaking nano titanium dioxide in 2mol/L sodium hydroxide solution, continuously stirring in the soaking process, and then washing with deionized water to be neutral;
b. soaking the washed nano titanium dioxide in 2mol/L acetic acid solution, carrying out ultrasonic oscillation treatment for 15-20min in the soaking process, drying at 50 ℃, mixing a silane coupling agent accounting for 0.5 percent of the weight of the nano titanium dioxide with the nano titanium dioxide, and grinding to fully and uniformly mix the nano titanium dioxide;
c. adding 5 times of water by weight of chitosan into the chitosan, dropwise adding glacial acetic acid into the water to adjust the pH value to 3-4, stirring to dissolve the chitosan, mixing the nano titanium dioxide prepared in the step b and the chitosan solution according to the weight ratio of 1:4, carrying out ultrasonic oscillation treatment for 15min, carrying out vacuum filtration, and drying to obtain modified nano titanium dioxide;
(2) spinning;
taking 100 parts by weight of polypropylene and 40 parts by weight of polyethylene glycol terephthalate, drying, adding 1-3 parts by weight of the modified nano titanium dioxide prepared in the step (1), mixing materials by using a double-screw extruder, and then spinning;
(3) opening;
opening and mixing the spinning in the step (2) by using an opener;
(4) carding;
carding the opened spinning;
(5) laying a net;
lapping the carded spinning by using a lapping machine, finishing and forming, carrying out spun-bonding by using a double-roller hot rolling machine, cooling and winding;
the roll shaft temperature of the double-roll hot rolling mill is 145 ℃;
after the spinning in the step (2), adding 10 parts of spinning into 100 parts of 1.2mol/L acetic acid solution, soaking at a constant temperature of 25 ℃ for 20min, introducing nitrogen to discharge oxygen in the system, adding 10 parts of ethyl acrylate ethanol solution with the mass fraction of 5%, uniformly stirring, slowly adding 0.015 part of potassium persulfate, stirring at a speed of 500r/min in the adding process, heating to 65 ℃, continuously stirring, reacting for 50min, cooling to normal temperature, adding 2mol/L sodium hydroxide solution to adjust the pH of the solution to 8.5, filtering the spinning, washing to be neutral, and drying to obtain modified spinning;
in step (5), the laid mesh is treated at 60 ℃ for 60min and then treated with a twin roll hot mill.
2. The method for preparing the novel non-woven fabric with the bacteriostatic action according to claim 1, which is characterized in that: the surface of the roller of the double-roller hot rolling mill is provided with needle-shaped burrs, and the lengths of the burrs are 0.1 mm.
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| CN201810928653.4A CN108978038B (en) | 2018-08-15 | 2018-08-15 | Preparation method of novel non-woven fabric with antibacterial effect |
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| CN110894642B (en) * | 2019-12-16 | 2021-06-22 | 中科纺织研究院（青岛）有限公司 | Chitin modified PP spunbonded non-woven fabric |
Citations (4)
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| CN102816349A (en) * | 2012-08-24 | 2012-12-12 | 浙江大学 | Chitosan/nano-TiO2 composite material and preparation method and application thereof |
| CN103184570A (en) * | 2013-04-09 | 2013-07-03 | 苏州维赛生物医药有限公司 | Silk-fibroin-based antibacterial nanofiber and preparation method thereof |
| CN105200856A (en) * | 2015-08-09 | 2015-12-30 | 浙江理工大学 | Chitosan/titanium dioxide nano-composite antibacterial coating preparation method |
| CN107227555A (en) * | 2017-07-21 | 2017-10-03 | 江苏科来材料科技有限公司 | A kind of nano modification melt-blown non-woven cloth material and its manufacture method |
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- 2018-08-15 CN CN201810928653.4A patent/CN108978038B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102816349A (en) * | 2012-08-24 | 2012-12-12 | 浙江大学 | Chitosan/nano-TiO2 composite material and preparation method and application thereof |
| CN103184570A (en) * | 2013-04-09 | 2013-07-03 | 苏州维赛生物医药有限公司 | Silk-fibroin-based antibacterial nanofiber and preparation method thereof |
| CN105200856A (en) * | 2015-08-09 | 2015-12-30 | 浙江理工大学 | Chitosan/titanium dioxide nano-composite antibacterial coating preparation method |
| CN107227555A (en) * | 2017-07-21 | 2017-10-03 | 江苏科来材料科技有限公司 | A kind of nano modification melt-blown non-woven cloth material and its manufacture method |
Non-Patent Citations (1)
| Title |
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| 聚丙烯/改性纳米二氧化钛复合材料的制备与性能;杨青等;《高分子材料科学与工程》;20090131;第25卷(第1期);第48-51页 * |
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Effective date of registration: 20201214 Address after: Dongju Road, Zhejiang Longyou Industrial Park, Longyou County, Quzhou City, Zhejiang Province Applicant after: Zhejiang falaifu non woven fabric Co.,Ltd. Address before: No.22, Zhangcun, Juxing administrative village, Qingxi Town, Hanshan County, Ma'anshan City, Anhui Province Applicant before: MAANSHAN ZHUOFAN NEW MATERIAL TECHNOLOGY Co.,Ltd. |
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