CN109620553B - Preparation method of graphene antibacterial hygienic product chip - Google Patents
Preparation method of graphene antibacterial hygienic product chip Download PDFInfo
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- CN109620553B CN109620553B CN201811335745.8A CN201811335745A CN109620553B CN 109620553 B CN109620553 B CN 109620553B CN 201811335745 A CN201811335745 A CN 201811335745A CN 109620553 B CN109620553 B CN 109620553B
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61F—FILTERS IMPLANTABLE INTO BLOOD VESSELS; PROSTHESES; DEVICES PROVIDING PATENCY TO, OR PREVENTING COLLAPSING OF, TUBULAR STRUCTURES OF THE BODY, e.g. STENTS; ORTHOPAEDIC, NURSING OR CONTRACEPTIVE DEVICES; FOMENTATION; TREATMENT OR PROTECTION OF EYES OR EARS; BANDAGES, DRESSINGS OR ABSORBENT PADS; FIRST-AID KITS
- A61F13/00—Bandages or dressings; Absorbent pads
- A61F13/15—Absorbent pads, e.g. sanitary towels, swabs or tampons for external or internal application to the body; Supporting or fastening means therefor; Tampon applicators
- A61F13/84—Accessories, not otherwise provided for, for absorbent pads
- A61F13/8405—Additives, e.g. for odour, disinfectant or pH control
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61F—FILTERS IMPLANTABLE INTO BLOOD VESSELS; PROSTHESES; DEVICES PROVIDING PATENCY TO, OR PREVENTING COLLAPSING OF, TUBULAR STRUCTURES OF THE BODY, e.g. STENTS; ORTHOPAEDIC, NURSING OR CONTRACEPTIVE DEVICES; FOMENTATION; TREATMENT OR PROTECTION OF EYES OR EARS; BANDAGES, DRESSINGS OR ABSORBENT PADS; FIRST-AID KITS
- A61F13/00—Bandages or dressings; Absorbent pads
- A61F13/15—Absorbent pads, e.g. sanitary towels, swabs or tampons for external or internal application to the body; Supporting or fastening means therefor; Tampon applicators
- A61F13/15577—Apparatus or processes for manufacturing
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61F—FILTERS IMPLANTABLE INTO BLOOD VESSELS; PROSTHESES; DEVICES PROVIDING PATENCY TO, OR PREVENTING COLLAPSING OF, TUBULAR STRUCTURES OF THE BODY, e.g. STENTS; ORTHOPAEDIC, NURSING OR CONTRACEPTIVE DEVICES; FOMENTATION; TREATMENT OR PROTECTION OF EYES OR EARS; BANDAGES, DRESSINGS OR ABSORBENT PADS; FIRST-AID KITS
- A61F13/00—Bandages or dressings; Absorbent pads
- A61F13/15—Absorbent pads, e.g. sanitary towels, swabs or tampons for external or internal application to the body; Supporting or fastening means therefor; Tampon applicators
- A61F13/84—Accessories, not otherwise provided for, for absorbent pads
- A61F13/8405—Additives, e.g. for odour, disinfectant or pH control
- A61F2013/8408—Additives, e.g. for odour, disinfectant or pH control with odour control
- A61F2013/8414—Additives, e.g. for odour, disinfectant or pH control with odour control with anti-microbic
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- Health & Medical Sciences (AREA)
- Engineering & Computer Science (AREA)
- General Health & Medical Sciences (AREA)
- Public Health (AREA)
- Heart & Thoracic Surgery (AREA)
- Vascular Medicine (AREA)
- Life Sciences & Earth Sciences (AREA)
- Animal Behavior & Ethology (AREA)
- Epidemiology (AREA)
- Biomedical Technology (AREA)
- Veterinary Medicine (AREA)
- Manufacturing & Machinery (AREA)
- Absorbent Articles And Supports Therefor (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
- Nonwoven Fabrics (AREA)
- Artificial Filaments (AREA)
Abstract
The invention discloses a preparation method of a graphene antibacterial hygienic product chip; the method comprises the following steps: mixing graphene, chitosan and zinc pyrithione to form a graphene antibacterial agent; uniformly mixing the graphene antibacterial agent and the polyacrylic acid solution, spinning to form antibacterial fibers, and mixing the antibacterial fibers and the water absorption fibers to prepare a first antibacterial non-woven fabric layer; mixing and melting a graphene antibacterial agent and polyethylene, extruding the mixture into filaments by a spinneret plate to prepare highly oriented fibers, distributing the highly oriented fibers on a net curtain, prepressing and shaping the fibers by a hot press roller to form a fiber net, and then carrying out hot rolling reinforcement to obtain a second antibacterial non-woven fabric layer; and compounding the first antibacterial non-woven fabric layer. The surface of the non-woven fabric layer in the chip is soft and fluffy, has excellent texture, has an antibacterial function, good water absorption and comfortableness, has high, lasting and safe broad-spectrum antibacterial performance, can be widely used for hygienic products, and is safe and sanitary.
Description
Technical Field
The invention relates to the technical field of graphene, in particular to a preparation method of a graphene antibacterial hygienic product chip.
Background
In the selection of fabrics of the sanitary products on the market, such as sanitary towels, panty liners, baby diapers and the like, chemical fiber fabrics are mainly used, and some products are pure cotton fabrics, fabrics containing bamboo fibers and fabrics containing silk. The functions of the traditional Chinese medicine preparation are mainly improved from the aspects of soft hand feeling, skin friendliness, moistening, moisture absorption, ventilation, dehumidification, heat dissipation, microcirculation promotion and the like, and the traditional Chinese medicine or antibacterial components (such as chlorhexidine products) are added to the traditional Chinese medicine preparation to achieve the functions of skin mucosa disinfection, antibiosis and the like.
Graphene is a two-dimensional crystal that is exfoliated from graphite to only one atomic thickness, about 0.34nm thick. The discovery of graphene in 2004 promoted research on carbon nanomaterials again, following the first reports of carbon nanotubes in 1985C 60 (fullerenes) and 1991. Researches show that the graphene has remarkable mechanical properties, conductivity, thermal properties, optical properties, high-efficiency antibacterial deodorization, antistatic and other properties. In order to put these excellent properties of graphene into practical use, further studies on graphene have been conducted.
Through the search of the existing patent documents, the Chinese patent application with the application publication number of CN 106581732A discloses a multifunctional graphene sanitary towel and a preparation method thereof; the powder solid bonded on the moxa sanitary napkin contains graphene oxide. However, the traditional Chinese medicine preparation is mainly utilized, and the problems of short storage period, easy deterioration and invalidation and the like exist; moreover, the graphene-containing powder solid is adhered to the moxa sanitary napkin, and the antibacterial component is easy to fall off to cause failure.
The utility model with the publication number of CN 206239604U discloses a sanitary towel structure with good antibacterial and bacteriostatic comfort; it lays warm fibre in graphite alkene (developing living beings graphite alkene from the corncob straw in the intermediate layer of sanitary towel body, again with the multi-functional fiber material of its and all kinds of fibre complex production), utilizes the characteristic that warm fibre has in the graphite alkene to guarantee the travelling comfort of sanitary towel in the use, prevents bacterial growing, adsorbs the peculiar smell, promotes blood circulation. However, the surface softness, bulkiness, water absorption, comfort and the like of fiber materials formed by compounding graphene and various fibers at present are not good, and the problems that antibacterial components are easy to fall off and lose efficacy, the antibacterial performance is unstable and the like exist, so that the popularization and the application of the fiber materials in hygienic products are seriously influenced.
Disclosure of Invention
The invention aims to overcome the technical defects of the antibacterial material, and provides a preparation method of a graphene antibacterial sanitary product chip by utilizing the characteristics of excellent antibacterial performance, no toxicity to human bodies and no stimulation to skin of graphene; and the chip is used for preparing the antibacterial chip which can be applied to the hygienic products. The antibacterial component of the antibacterial chip is not easy to fall off, and the antibacterial component can be slowly released to generate an antibacterial effect for a long time.
The purpose of the invention is realized by the following technical scheme:
the invention relates to a preparation method of a graphene antibacterial hygienic product chip, which comprises the following steps:
s1, mixing graphene, chitosan and zinc pyrithione in a mass ratio of 1-12: 10-15: 3-5 to form a graphene antibacterial agent;
s2, adding the graphene antibacterial agent into a polyacrylic acid solution, uniformly mixing, and spinning to form antibacterial fibers; the mass ratio of the graphene antibacterial agent to the polyacrylic acid solution is 15-30: 20-40; the mass percentage concentration of the polyacrylic acid solution is 40-60%;
s3, uniformly mixing the antibacterial fibers and the water-absorbing fibers in a mass ratio of 35-70: 40-60, and sequentially opening, carding, lapping and needling to form a first antibacterial non-woven fabric layer;
s4, adding the graphene antibacterial agent and polyethylene into a screw extruder, mixing and melting; the mass ratio of the graphene antibacterial agent to the polyethylene is 10-20: 60-80;
s5, distributing the melt obtained in the step S4 by a spinning manifold so that the melt is uniformly distributed on the whole width, and extruding the fluid melt into filaments by a spinneret plate by a spinning assembly; after cooling, drafting the melt stream to make the melt stream into highly oriented fibers;
s6, distributing the fibers on a net curtain, and prepressing and shaping the fibers through a hot-press roller to form a fiber net; the fiber net is sent to a net curtain to be subjected to hot rolling reinforcement to obtain a second antibacterial non-woven fabric layer;
and S7, carrying out composite spunlace treatment on the first antibacterial non-woven fabric layer and the second antibacterial non-woven fabric layer, and drying to obtain the chip.
Preferably, in step S1, the graphene includes one or more of graphene prepared by a vapor deposition method, carbon dioxide supercritical expansion exfoliated graphene, chemically oxidized exfoliated graphene, coupling agent modified graphene oxide, amino polymer modified graphene oxide, cationic surfactant modified graphene oxide, bromododecane modified graphene oxide, bromohexadecane modified graphene oxide, bromooctadecane modified graphene oxide, reduced graphene oxide obtained by high-temperature thermal expansion, reduced graphene oxide obtained by low-temperature thermal expansion, graphene obtained by electrochemical exfoliation, modified electrochemical exfoliated graphene, mechanical ball milling exfoliated graphene, and three-roll grinding mechanical exfoliated graphene.
Preferably, in step S3, the water-absorbing fibers include one or more of natural fibers, cellulose fibers, polypropylene fibers, polyacrylonitrile fibers, and polyvinyl alcohol fibers.
Preferably, in step S4, the polyethylene has a number average molecular weight of 2000 to 3000 g/mol.
Preferably, in step S4, the melting is performed by heating to 100-120 ℃ after mixing, heating for 20-40S, heating to 160-170 ℃ for 15-25S, and finally heating to 200-220 ℃ for 3-7S.
Preferably, in step S5, the temperature in the spinning box during extrusion into filaments is 180 to 220 ℃.
Preferably, in step S6, the temperature for pre-pressing and shaping by the hot press roller is 80 to 100 ℃.
Preferably, in step S6, the hot rolling strengthening temperature is 150 to 170 ℃.
Preferably, in step S7, the complex spunlace process includes the steps of opening and mixing, carding, cross-lapping, drafting, pre-wetting, forward and reverse spunlacing, post-finishing, drying, and winding.
Preferably, in the step S7, the drying temperature is 60 to 90 ℃.
Compared with the prior art, the invention has the beneficial effects that:
1. the antibacterial component in the graphene antibacterial hygienic product chip is not easy to fall off, the antibacterial component can be slowly released, the antibacterial effect is generated for a long time, and the antibacterial rate reaches more than 99.9%;
2. the surface of the non-woven fabric layer in the graphene antibacterial hygienic product chip is soft and fluffy, has excellent texture, has an antibacterial function, good water absorption and comfortableness, and high, lasting and safe broad-spectrum antibacterial performance, can be widely used for hygienic products, and is safe and sanitary.
Detailed Description
The present invention will be described in detail with reference to examples. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that it would be apparent to those skilled in the art that several modifications and improvements can be made without departing from the inventive concept. All falling within the scope of the present invention.
Example 1
The embodiment relates to a preparation method of a graphene antibacterial hygienic product chip; the method comprises the following specific steps:
(1) mixing graphene, chitosan and zinc pyrithione in a mass ratio of 6:13:4 to prepare a graphene antibacterial agent, adding the prepared antibacterial agent into a polyacrylic acid solution (the mass ratio of the graphene antibacterial agent to the polyacrylic acid solution is 22:25, and the mass percentage concentration of the polyacrylic acid solution is 50%), uniformly mixing, spinning to form antibacterial fibers, uniformly mixing the antibacterial fibers and water-absorbing fibers in a mass ratio of 50:50, and sequentially opening, carding, lapping and needling to form a first antibacterial non-woven fabric layer;
(2) adding a graphene antibacterial agent and polyethylene (molecular weight of 2000-3000) in a mass ratio of 15:70 into a screw extruder, primarily mixing, raising the temperature to 110 ℃, heating for 30s, raising the temperature to 165 ℃, heating for 20s, finally raising the temperature to 210 ℃, and heating for 6s for melting to fully mix the materials;
(3) distributing the melt in the step (3) by using a spinning manifold so that the melt is distributed on the whole width as uniformly as possible, extruding the fluid melt into filaments by using a spinneret plate by using a spinning assembly, wherein the temperature in the spinning manifold is 200 ℃;
(4) after cooling, drafting the melt trickle by using high-speed airflow generated by a fan to enable the melt trickle to become highly oriented fibers, then randomly distributing the fibers on a net curtain, forming a fiber net by pre-pressing and shaping a hot-pressing roller with the temperature of 90 ℃, and sending the fiber net to a hot-rolling mill with the temperature of 160 ℃ by the net curtain for further reinforcement to obtain a second antibacterial non-woven fabric layer;
(5) and carrying out composite spunlace treatment on the first antibacterial non-woven fabric layer and the second antibacterial non-woven fabric layer, and drying to obtain a graphene antibacterial chip finished product.
Example 2
The embodiment relates to a preparation method of a graphene antibacterial hygienic product chip; the specific steps are the same as those in the embodiment 1, except that:
(1) the mass ratio of graphene to chitosan to zinc pyrithione in the graphene antibacterial agent is 1:10: 3; the mass ratio of the graphene antibacterial agent to the polyacrylic acid solution is 15: 20; the mass ratio of the antibacterial fiber to the water-absorbing fiber is 35: 40;
(2) the mass ratio of the graphene antibacterial agent to the polyethylene is 10: 60; after primary mixing, raising the temperature to 100 ℃, heating for 40s, raising the temperature to 160 ℃, heating for 25s, finally raising the temperature to 200 ℃, and heating for 7s for melting;
(3) the temperature in the spinning box is 180 ℃;
(4) the temperature for hot-press roller prepressing and shaping is 80 ℃; the temperature for hot rolling consolidation was 150 ℃.
Example 3
The embodiment relates to a preparation method of a graphene antibacterial hygienic product chip; the specific steps are the same as those in the embodiment 1, except that:
(1) the mass ratio of graphene to chitosan to zinc pyrithione in the graphene antibacterial agent is 12:15: 5; the mass ratio of the graphene antibacterial agent to the polyacrylic acid solution is 30: 40; the mass ratio of the antibacterial fiber to the water-absorbing fiber is 70: 60;
(2) the mass ratio of the graphene antibacterial agent to the polyethylene is 20: 80; after primary mixing, raising the temperature to 120 ℃, heating for 20s, raising the temperature to 170 ℃, heating for 15s, finally raising the temperature to 220 ℃, and heating for 3s for melting;
(3) the temperature in the spinning box is 220 ℃;
(4) the temperature for hot-press roller prepressing and shaping is 100 ℃; the temperature of hot rolling consolidation was 170 ℃.
Comparative example 1
The comparative example relates to a preparation method of a graphene antibacterial hygienic product chip; the specific steps are the same as those in the embodiment 1, except that:
the chip comprises only a first antibacterial non-woven fabric layer.
Comparative example 2
The comparative example relates to a preparation method of a graphene antibacterial hygienic product chip; the specific steps are the same as those in the embodiment 1, except that:
the chip comprises only a second antimicrobial nonwoven fabric layer.
Comparative example 3
The comparative example relates to a preparation method of a graphene antibacterial hygienic product chip; the method comprises the following specific steps:
(1) under the condition that the power is 90W, 50mg of graphene oxide is dissolved in 100ml of absolute ethyl alcohol to prepare a graphene oxide solution.
(2) Adding 5g of polypropylene into 80g of dimethylbenzene, heating and dissolving in a three-neck flask at the stirring speed of 800r/min at the temperature of 125 ℃, and dissolving the polypropylene in a dimethylbenzene solvent to obtain a polypropylene solution.
(3) Heating to 155 ℃, adding a small amount of graphene oxide solution into the polypropylene solution in batches, stirring for 0.5h, uniformly mixing, and drying the mixture in an air atmosphere at 50 ℃ for 48h to obtain a graphene oxide modified polypropylene composite material; the composite material is then melt spun. And preparing the graphene antibacterial hygienic product chip.
The graphene antibacterial chip is subjected to testing of softness, bulkiness, water absorption, antibacterial property and the like of the surface of the material, wherein the antibacterial property is tested according to ASTM-E2149-13a, and the testing results are shown in Table 1:
TABLE 1
The foregoing description of specific embodiments of the present invention has been presented. It is to be understood that the present invention is not limited to the specific embodiments described above, and that various changes and modifications may be made by one skilled in the art within the scope of the appended claims without departing from the spirit of the invention.
Claims (2)
1. A preparation method of a graphene antibacterial hygienic product chip is characterized by comprising the following steps:
s1, mixing graphene, chitosan and zinc pyrithione in a mass ratio of 1-12: 10-15: 3-5 to form a graphene antibacterial agent;
s2, adding the graphene antibacterial agent into a polyacrylic acid solution, uniformly mixing, and spinning to form antibacterial fibers; the mass ratio of the graphene antibacterial agent to the polyacrylic acid solution is 15-30: 20-40; the mass percentage concentration of the polyacrylic acid solution is 40-60%;
s3, uniformly mixing the antibacterial fibers and the water-absorbing fibers in a mass ratio of 35-70: 40-60, and sequentially opening, carding, lapping and needling to form a first antibacterial non-woven fabric layer;
s4, adding the graphene antibacterial agent and polyethylene into a screw extruder, mixing and melting; the mass ratio of the graphene antibacterial agent to the polyethylene is 10-20: 60-80;
s5, distributing the melt obtained in the step S4 by a spinning manifold so that the melt is uniformly distributed on the whole width, and extruding the fluid melt into filaments by a spinneret plate by a spinning assembly; after cooling, drafting the melt stream to make the melt stream into highly oriented fibers;
s6, distributing the fibers on a net curtain, and prepressing and shaping the fibers through a hot-press roller to form a fiber net; the fiber net is sent to a net curtain to be subjected to hot rolling reinforcement to obtain a second antibacterial non-woven fabric layer;
s7, carrying out composite spunlace treatment on the first antibacterial non-woven fabric layer and the second antibacterial non-woven fabric layer, and drying to obtain the chip; the drying temperature is 60-90 ℃;
in step S1, the graphene includes one or more of a vapor deposition method for preparing graphene, carbon dioxide supercritical expansion exfoliated graphene, chemical oxidation exfoliated graphene oxide, coupling agent modified graphene oxide, amino polymer modified graphene oxide, cationic surfactant modified graphene oxide, bromododecane modified graphene oxide, bromohexadecane modified graphene oxide, bromooctadecane modified graphene oxide, reduced graphene oxide obtained by high-temperature thermal expansion, reduced graphene oxide obtained by low-temperature thermal expansion, graphene obtained by electrochemical exfoliation, modified electrochemical exfoliated graphene, mechanical ball milling exfoliated graphene, and three-roll grinding mechanical exfoliated graphene;
in step S3, the water-absorbing fibers include one or more of natural fibers, cellulose fibers, polypropylene fibers, polyacrylonitrile fibers, and polyvinyl alcohol fibers;
in the step S4, the melting step is to heat the mixture to 100-120 ℃ for 20-40S, then to 160-170 ℃ for 15-25S, and finally to 200-220 ℃ for 3-7S;
in the step S5, the temperature in a spinning box is 180-220 ℃ when the extruded filaments are formed;
in the step S6, the temperature for hot press roller prepressing and shaping is 80-100 ℃;
in step S6, the temperature of the hot rolling reinforcement is 150-170 ℃.
2. The method for preparing the graphene antibacterial sanitary chip according to claim 1, wherein in step S4, the number average molecular weight of the polyethylene is 2000-3000 g/mol.
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| CN111449847A (en) * | 2020-04-22 | 2020-07-28 | 上海紫河生物科技有限公司 | Bacteriostatic sanitary towel |
| CN112899880A (en) * | 2021-02-07 | 2021-06-04 | 郝宝民 | Graphene non-woven fabric and preparation method thereof |
| EP4190293B1 (en) * | 2021-12-01 | 2024-07-03 | Fameccanica.Data S.p.A. | A washable absorbent garment, method and apparatus for producing the same |
| CN116531181B (en) * | 2023-05-09 | 2024-02-20 | 东莞苏氏卫生用品有限公司 | Five-layer laminated structure composite fiber core body and manufacturing method thereof |
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| US9591853B2 (en) * | 2013-01-07 | 2017-03-14 | Ramot At Tel-Aviv University Ltd. | Jellyfish-derived polymer |
| US20180036341A1 (en) * | 2016-08-02 | 2018-02-08 | Linkwin Technology Co., Ltd. | Method of using carbonized material to inhibit bacteria |
| CN206239604U (en) * | 2016-08-29 | 2017-06-13 | 王志全 | A kind of good SANITARY NAPKIN CONSTRUCTION of antibacterial bacteriostatic comfortableness |
| CN206566092U (en) * | 2016-11-30 | 2017-10-20 | 济南圣岱尔电子商务有限公司 | A kind of sanitary napkin of graphene non-woven fabric |
| CN108248168A (en) * | 2016-12-28 | 2018-07-06 | 天津圣奥无纺布有限公司 | A kind of antibacterial nonwoven cloth and preparation method thereof |
| CN107460559A (en) * | 2017-09-05 | 2017-12-12 | 福州市晋安区技智企业管理咨询有限公司 | A kind of preparation method of graphene polyester fiber |
| CN108720998A (en) * | 2018-06-06 | 2018-11-02 | 张小伏 | A kind of speed suction high air permeable sanitary towel of antibacterial |
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