CN103835124B - Carry silver-colored COTTON FABRIC anti-biotic material and preparation method thereof - Google Patents
Carry silver-colored COTTON FABRIC anti-biotic material and preparation method thereof Download PDFInfo
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- CN103835124B CN103835124B CN201410069747.2A CN201410069747A CN103835124B CN 103835124 B CN103835124 B CN 103835124B CN 201410069747 A CN201410069747 A CN 201410069747A CN 103835124 B CN103835124 B CN 103835124B
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Abstract
To the invention discloses with pure cotton cloth in COTTON FABRIC and cotton blended cloth as brocade cotton, polyester-cotton blend, cotton wash Ag-carried antibacterial material and preparation method thereof into matrix, belong to functional high molecule material technical field.Silver is dispersed with equably in the fiber reinforcement of such antibacterial cotton fabric.Its preparation method is: wash with after nonionic surface active agent process by pure cotton cloth in COTTON FABRIC, brocade cotton, polyester-cotton blend, cotton, in immersion silver ammino solution, adds after thermal response terminates, reduces, make to be dispersed with silver equably in cotton-textile fibres skeleton with reductant.The easy easy control of preparation method, reaction condition be gentle, consuming time short, consume energy low, low-carbon environment-friendly, reaction reagent toxicity used is low, environmental friendliness.Such year silver-colored COTTON FABRIC, can Chinese People's Anti-Japanese Military and Political College enterobacteria and staphylococcus aureus well through transshipping after silver.
Description
Technical field
The present invention relates to a kind of high-molecular anti-bacteria material, particularly relate to a kind of year silver-colored COTTON FABRIC anti-biotic material, belong to functional high polymer material field.
Background technology
The function of anti-biotic material is mainly manifested in and suppresses or kill pathogenic bacteria and mould, blocks transmission.Silver or silver ion there is good anti-microbial property, in the time immemorial generation by people are found, as people with silverware ware splendid attire food to prevent from going rotten.20 beginnings of the century, the antibiotic property good due to silver and anti-infection property, silver system anti-biotic material is widely used in clinical medicine.At present, most of Ag-carried antibacterial material by diverse ways, silver ion is incorporated into carrier surface with certain carrier (as silica gel, zeolite, activated alumina, basic zirconium phosphate, imvite, hydroxyapatite, natural or chemical fibre etc.), thus obtain anti-biotic material.As silver-carrying active aluminum oxide (ZL200610068586), silver-zirconium phosphate antimicrobial (CN201210273501), silicon-zinc mesoporous material or silica carrying silver antimicrobials (CN200910156604, CN201210062784), sliver-carried nano-montmorillonite (ZL200910303849, CN201010571408), super-fine fly ash silver-loaded antimicrobial (CN200910177165), argentum-carried hydroxylapatite (CN200810152897), zeolite with carrying silver (CN201010550378) and perovskite-type compounds carry silver (ZL200610032880), silver-plated cotton fiber (CN201120511906, CN201120511907) and chemical fibre Ag-carried antibacterial material as CN201210078915 etc.
Wherein, silver-contained antibacterial fiber/fibre due to its by silver or silver ion load on fibrous material, while the anti-microbial property had, the advantage of fibrous material can be played, as the breeding owing to being particularly suitable for bacterium in clothes and bed clothes, antibacterial fiber product is therefore used just can directly to prevent or effectively eliminate the breeding of bacterium; Secondly, the performance of fiber self can be safeguarded, the antibacterial and antimildew function had as anti-bacterial fibre self then can prevent the changing color of textile caused by bacterium effectively, the brittle situation jeopardizing human body skin such as rotten occurs; Again, belong to the antibacterial or sterilization of original position in the antibacterial process of antibacterial fiber material/goods, do not need other external energy.These advantages impel silver-contained antibacterial fiber material and goods thereof to be widely used in the industry such as civilian, military, medical.
The preparation method of silver-contained antibacterial fiber material mainly contains: (1) at fibrillation electroplate as ZL200410024079.8 and CN01114999.X etc.; (2) by other fibers and silver-colored fiber blend as ZL201110084108.X, CN201120079321, CN201310307066.0 etc.; (3), after antiseptic being disperseed, be carried on fiber by the method for dipping or slurry parcel.As CN201210078915, CN201110204640, CN103266467A etc.(4) method of electrostatic spinning.As XiongliXu, etc. (FibersandPolymers, 2008,9:685-690); ShanWang, etc. (ColliodPolymerScience, 2012,290:667-672); HanyS.Abdo, etc. (FibersandPolymers, 2013,14:1985-1992) with the method for electrostatic spinning respectively on gelatin fiber, carbon fiber and beta-cyclodextrin/polyvinyl pyrrolidone fibers matrix carrying nano silver prepare anti-biotic material.
In above-mentioned silver-contained antibacterial fiber material, because cotton fiber belongs to natural fiber material, be that carrier prepares Ag-carried antibacterial material with cotton fiber, the danger of other harmful chemical components of matrix material stripping is not had in use procedure, (structure and the antibiotic property of silver-colored cotton yarn is carried as occupied quiet rosy clouds etc., printing and dyeing, 2006,23:8-10; Alkali treatment cotton yarn carries silver process and Research on antibacterial thereof, printing and dyeing assistant, 2005,12:13-15) by normal temperatures by cotton yarn directly or immerse silver ammino solution after alkali treatment, be then that reductant reduces with tannic acid, a preparation year silver-colored cotton yarn.Adsorption For Ag after cotton fiber and glyceral methacrylate-aminodiacetic acid chelating is prepared Ag-carried antibacterial material by Chuh-YeanChen, etc. (MaterialsLetters, 2008,62:3607-3609); Cotton fiber immerses in KOH-AgNO3 solution by MohammadShateriKhalil-Abad, etc. (JournalofColloidandInterfaceScience, 2010,351:293-298), obtains carrying silver-colored cotton fiber by Vc in-situ reducing.JuyoungKimetetc. cotton balls is immersed AgCl-NH by (JournalofBiologicalEngineering, 2009,3:20-29)
4gossypin-OAg anti-biotic material is obtained in OH solution.At present, document or patent are that matrix carries silver mainly with cotton fiber greatly, and investigating cotton fiber goods, to carry silvery very few for the report of anti-biotic material.Because cotton fiber goods have moisture absorption and good permeability, soft and warming characteristic, after COTTON FABRIC directly carries silver, just can be directly used in antibacterial occasion, and the problem that after need not considering antibiotic cotton fiber weaving reprocessing again, whether anti-microbial property reduces.And, because cotton is in the process of spinning into cloth, need the monomer adding PMA, acrylamide-vinyl acetate and so on, these monomers directly affect the further reaction kinetic of COTTON FABRIC, as affected the load efficiency of functionalization ion and being uniformly distributed, this makes the reaction difficulty of the more simple cotton fiber functionalization of COTTON FABRIC functionalization strengthen.Therefore, silver-colored COTTON FABRIC is carried in research and development, while making full use of COTTON FABRIC intrinsic advantage, also to fully take into account the negative effect that suitable technology of preparing is brought to solve monomer, the silver-colored COTTON FABRIC of carrying of gained can be made like this to have higher actual use value.
Summary of the invention
The object of the present invention is to provide a kind of anti-microbial property good, take COTTON FABRIC as the Ag-carried antibacterial material of carrier; Another object of the present invention is to provide its preparation method.
For realizing the object of the invention, wash as matrix material with pure cotton cloth in COTTON FABRIC and blending cotton such as brocade cotton, polyester-cotton blend, cotton, by gentleness, easy easy control, short, eco-friendly synthetic route consuming time, the Ag-carried antibacterial COTTON FABRIC that preparation silver is evenly distributed, anti-microbial property is good is to realize technical solution of the present invention.
Its synthetic method is: COTTON FABRIC washed, and immerses (solid-to-liquid ratio is 1:10-30) in the non-ionic surface active agent of mass percent 1% ~ 5% and fully soaks 30 ~ 60min.The ammoniacal liquor of 5% ~ 30% is added, the silver ammino solution of obtained clarification in the liquor argenti nitratis ophthalmicus of 0.1 ~ 1M.COTTON FABRIC after soaking immersed in silver ammino solution (solid-to-liquid ratio is 1:10-30), 30 ~ 70 DEG C add thermal response 15 ~ 60mins.After reaction terminates, take out year silver-colored COTTON FABRIC distilled water and clean, put into reductant reaction 1 ~ 2 hour (solid-to-liquid ratio is 1:10-30) of mass percent 1% ~ 10%, after reaction terminates, with distilled water cleaning, dry.
The present invention's COTTON FABRIC used is that commercial goods level pure cotton cloth and blending cotton such as brocade cotton, polyester-cotton blend, cotton are washed.Non-ionic surface active agent used is polyoxyethylene carboxylate.Reductant used is glucose.
Beneficial effect of the present invention is: (1) overcomes added monomer in COTTON FABRIC fabrication processes and, to the negative effect of carrying silver, prepared the Ag-carried antibacterial COTTON FABRIC of good combination property.(2) after COTTON FABRIC carries silver, can directly be processed into clothes, medical antibacterial articles for use etc., without the need to weaving through secondary, and COTTON FABRIC is natural environmental-protective product again, and Ag-carried antibacterial COTTON FABRIC effectively prevent the danger of matrix material harmful substance stripping.(3) COTTON FABRIC used is commercial goods, and raw material sources is extensive, and performance quality is stablized.(4) carry the easy easy control of silver-colored COTTON FABRIC preparation method, reaction condition gentle, consuming time short, consume energy low, low-carbon environment-friendly, is applicable to large-scale production.(5) do not add other organic crosslinking agents or reinforcing agent in course of reaction, avoid the pollution of toxic reagent, environmental friendliness.(6) that is prepared by the method carries silver-colored COTTON FABRIC, and silver is evenly distributed, and anti-microbial property is good, stable.
Accompanying drawing explanation
Fig. 1: SEM photo (amplifying 15000 times) (a: carry silver-colored pure cotton cloth of year silver-colored COTTON FABRIC that the present invention obtains; B: carry silver brocade cotton; C: carry silver-colored polyester-cotton blend; D.: carry silver-colored cotton and wash);
Fig. 2: what the embodiment of the present invention 1 was obtained carry silver-colored pure cotton cloth is to the inhibition zone control experiment of Escherichia coli and staphylococcus aureus; (a: pure cotton cloth is tested Escherichia coli; B: year silver-colored pure cotton cloth that the embodiment of the present invention 1 obtains is tested Escherichia coli; C: pure cotton cloth is tested staphylococcus aureus; D: year silver-colored pure cotton cloth that the embodiment of the present invention 1 obtains is tested staphylococcus aureus)
Fig. 3: what the present invention obtained carries the antibiotic rate of silver-colored COTTON FABRIC to Escherichia coli and staphylococcus aureus; (Fig. 3 a: carry silver-colored COTTON FABRIC to Escherichia coli, in figure
; Fig. 3 b: carry silver-colored COTTON FABRIC to staphylococcus aureus, in figure
);
Fig. 4: what the present invention obtained carries the antibiotic rate of silver-colored COTTON FABRIC to Escherichia coli and staphylococcus aureus after washing powder washing.(Fig. 4 a: carry silver-colored COTTON FABRIC to Escherichia coli, in figure
; Fig. 4 b: carry silver-colored COTTON FABRIC to staphylococcus aureus, in figure
).
Detailed description of the invention
For the present invention is described in detail better, as follows for embodiment:
Embodiment 1:
5g pure cotton cloth (containing cotton 100%), after distilled water cleaning, immerses in the polyoxyethylene carboxylate solution of 50ml mass percent 2%, takes out after 30min.At the AgNO of 0.1M
3the ammoniacal liquor of mass percent 20% is added, the silver ammino solution of obtained clarification in solution.COTTON FABRIC after soaking immersed in 100ml silver ammino solution, 40 DEG C add thermal response 30min.After reaction terminates, carry silver-colored COTTON FABRIC with distilled water cleaning, put into the glucose solution of 150ml mass percent 1%, after 60min, use distilled water clean surface, 30 DEG C of oven dry.Fig. 1 is the SEM photo carrying silver-colored pure cotton cloth, and as can be seen from Fig. 1 a, silver is distributed in cotton fiber equably.
Embodiment 2:
5g brocade cotton (containing cotton 75%, polyamide fibre 25%), after distilled water cleaning, immerses in the polyoxyethylene carboxylate solution of 50ml mass percent 2%, takes out after 30min.At the AgNO of 0.3M
3the ammoniacal liquor of mass percent 25% is added, the silver ammino solution of obtained clarification in solution.COTTON FABRIC after soaking immersed in 100ml silver ammino solution, 50 DEG C add thermal response 45min.After reaction terminates, carry silver-colored COTTON FABRIC with distilled water cleaning, put into the glucose solution of 150ml mass percent 3%, after 60min, use distilled water clean surface, 30 DEG C of oven dry.Fig. 1 carries the cotton SEM photo of silver brocade, and as can be seen from Fig. 1 b, silver is evenly distributed in bright and beautiful cotton fiber.
Embodiment 3:
5g polyester-cotton blend (containing cotton 33%, terylene 67%), after distilled water cleaning, immerses in the polyoxyethylene carboxylate solution of 50ml mass percent 5%, takes out after 30min.At the AgNO of 1M
3the ammoniacal liquor of mass percent 30% is added, the silver ammino solution of obtained clarification in solution.COTTON FABRIC after soaking immersed in 100ml silver ammino solution, 70 DEG C add thermal response 35min.After reaction terminates, carry silver-colored COTTON FABRIC with distilled water cleaning, put into the glucose solution of 150ml mass percent 7%, after 60min, use distilled water clean surface, 30 DEG C of oven dry.Fig. 1 is the SEM photo carrying silver-colored polyester-cotton blend, and as can be seen from Fig. 1 c, silver is evenly distributed in polyester fiber.
Embodiment 4:
5g cotton is washed (containing cotton 65%, terylene 35%), after distilled water cleaning, immerses in the polyoxyethylene carboxylate solution of 50ml mass percent 3%, takes out after 30min.At the AgNO of 0.5M
3the ammoniacal liquor of mass percent 30% is added, the silver ammino solution of obtained clarification in solution.COTTON FABRIC after soaking immersed in 100ml silver ammino solution, 60 DEG C add thermal response 50min.After reaction terminates, carry silver-colored COTTON FABRIC with distilled water cleaning, put into the glucose solution of 150ml mass percent 5%, after 60min, use distilled water clean surface, 35 DEG C of oven dry.Fig. 1 is the SEM photo that year silver-colored cotton is washed, and as can be seen from Fig. 1 d, silver is evenly distributed in cotton and washs in fiber.
Application examples 1:
Prepared by Example 1 carries silver-colored cotton (parallel get four parts), measures the antibacterial ability of this material to Escherichia coli and staphylococcus aureus with inhibition zone method.As shown in Figure 2, the inhibition zone size of formation is respectively 13mm and 11mm, illustrates that carrying silver-colored cotton has good Chinese People's Anti-Japanese Military and Political College enterobacteria and staphylococcus aureus performance.
Application examples 2:
Carry silver-colored COTTON FABRIC respectively in Example 1 ~ 4, (Fig. 3 a) and the antibiotic rate of staphylococcus aureus (Fig. 3 b) to Escherichia coli to measure it by shake flasks method.As shown in Figure 3 a, when contacting >=4 hours, four kinds carry silver-colored COTTON FABRIC to colibacillary antibiotic rate all more than 95%; As shown in Figure 3 b, be 6 constantly little when contacting, four kinds carry silver-colored COTTON FABRIC to the antibiotic rate of staphylococcus aureus all more than 90%.
Application examples 3:
Silver-colored COTTON FABRIC will be carried in application examples 2 after antibacterial, after washing powder cleaning, 35 DEG C of oven dry, again with shake flasks method measure its to Escherichia coli (Fig. 4 a) with the antibiotic rate (Fig. 4 b) of staphylococcus aureus.Through 25 times antibacterial-washing-antibacterial after, as shown in fig. 4 a, be 6 hours when contacting, four kinds carry silver-colored COTTON FABRIC and still can reach more than 95% to colibacillary antibiotic rate, as shown in Figure 4 b, be 6 constantly little when contacting, four kinds carry silver-colored COTTON FABRIC and still can reach more than 90% to the antibiotic rate of staphylococcus aureus.
Claims (3)
1. year silver-colored COTTON FABRIC anti-biotic material, it is characterized in that: be prepared from by being loaded into silver in the fiber reinforcement of COTTON FABRIC, concrete steps are as follows: COTTON FABRIC is washed, immersing in the non-ionic surface active agent of mass percent 1% ~ 5%, solid-to-liquid ratio is 1:10-30, fully soaks 30 ~ 60min; The ammoniacal liquor of mass percent 5% ~ 30% is added, the silver ammino solution of obtained clarification in the liquor argenti nitratis ophthalmicus of 0.1 ~ 1M; COTTON FABRIC after soaking immersed in silver ammino solution, solid-to-liquid ratio is 1:10-30, and 30 ~ 70 DEG C add thermal response 15 ~ 60mins; After reaction terminates, take out year silver-colored COTTON FABRIC distilled water and clean, the reductant putting into mass percent 1% ~ 10% reacts 1 ~ 2 hour, and solid-to-liquid ratio is 1:10-30, after reaction terminates, with distilled water cleaning, dries; Non-ionic surface active agent used is polyoxyethylene carboxylate; Reductant used is glucose.
2. as claimed in claim 1 carry silver-colored COTTON FABRIC anti-biotic material, it is characterized in that: COTTON FABRIC used is that in pure cotton cloth or blending cotton, cotton, the polyester-cotton blend of brocade or cotton are washed.
3. preparation method of carrying silver-colored COTTON FABRIC anti-biotic material as claimed in claim 1 or 2, it is characterized in that: realize as follows: COTTON FABRIC is washed, immerse in the non-ionic surface active agent of mass percent 1% ~ 5%, solid-to-liquid ratio is 1:10-30, fully soaks 30 ~ 60min; The ammoniacal liquor of mass percent 5% ~ 30% is added, the silver ammino solution of obtained clarification in the liquor argenti nitratis ophthalmicus of 0.1 ~ 1M; COTTON FABRIC after soaking immersed in silver ammino solution, solid-to-liquid ratio is 1:10-30, and 30 ~ 70 DEG C add thermal response 15 ~ 60mins; After reaction terminates, take out year silver-colored COTTON FABRIC distilled water and clean, the reductant putting into mass percent 1% ~ 10% reacts 1 ~ 2 hour, and solid-to-liquid ratio is 1:10-30, after reaction terminates, with distilled water cleaning, dries; Non-ionic surface active agent used is polyoxyethylene carboxylate; Reductant used is glucose.
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