CN102373618B - Silver-carried alginic acid fiber and preparation method thereof - Google Patents
Silver-carried alginic acid fiber and preparation method thereof Download PDFInfo
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- CN102373618B CN102373618B CN 201110366674 CN201110366674A CN102373618B CN 102373618 B CN102373618 B CN 102373618B CN 201110366674 CN201110366674 CN 201110366674 CN 201110366674 A CN201110366674 A CN 201110366674A CN 102373618 B CN102373618 B CN 102373618B
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Abstract
The invention relates to a medical disinfecting and sterilizing dressing raw material and a preparation method thereof, in particular to a silver-carried alginic acid fiber and a preparation method thereof. The preparation method comprises the following steps of: impregnating the alginic acid fiber in a water solution of nano silver with the concentration of 20-1000 ug/L, wherein the bath ratio is 1:10-200, and the impregnation time is 2-60 min; than, taking out the silver-carried alginic acid fiber absorbing elementary silver particles in an enrichment method, washing and drying the silver-carried alginic acid fiber through a water solution of organic solvent to obtain an alginic acid fiber with 0.01-4% of silver by weight and having good bulkiness and strong sterilization effect. The preparation method of the alginic acid fiber absorbing silver in an enrichment method provided by the invention has simple and feasible process, safe and nontoxic production process and practical application value.
Description
Technical field
The present invention relates to a kind of medical disinfecting sterilization dressing raw material and preparation method thereof, relate in particular to a kind of year silver-colored alginic acid fibre and preparation method thereof.
Background technology
Excellent medical material characteristics such as alginic acid fibre is good with its high-hygroscopicity that has, oxygen flow gas, good biocompatibility, biodegradable absorbability are used widely as hospital gauze, dressing etc. in medical industry.Alginic acid fibre hospital gauze, dressing have very strong anastalsis, can be in time the diffusate of wound be absorbed, but the wound that diffusate is many is relatively moister, the probability that infects is also bigger, by in alginic acid fibre, adding silver ion, can make the alginic acid medical dressing when having high-hygroscopicity, also have the excellent antibiotic performance with anti-microbial property.Silver-colored alginic acid fibre is carried in preparation probably two kinds usually: a kind of is to add in alginic acid fibre spinning solution or coagulating bath, as in the alginic acid fibre spinning solution, adding sodium sulfadiazine, silver nitrate, make the particle that contains flamazine in the spinning solution, or in spinning solution, directly add the basic zirconium phosphate sodium salt nano-powder of argentiferous, organizine obtains to carry silver-colored alginic acid fibre, as document " preparation method of silver-containing alginic acid fiber and performance " ([J] textile journal, 2005,7 (2): 126～128), reported silver nitrate is directly added in the alginic acid fibre spinning coagulation bath calcium chloride water that the method for silver-colored alginic acid fibre is carried in preparation; Another kind is to add in the back process of alginic acid fibre, Chinese invention patent " simple and easy method of alginic acid fibre quickly adding silver ion for sterilization " (CN101187153) in, disclose and a kind ofly alginic acid fibre impregnated in the sodium carboxymethylcellulose half sticky shape colloidal solution that contains silver ion, after dewater, simple and easy method that drying is made alginic acid fibre dressing, but in actual production, adopt the dressing of the method alginic acid fibre very easily to harden, and handle inhomogeneous; Disclosing a kind of nanometer silver paste with 0.01～1% as Chinese invention patent (CN1935268) directly sprays, make nano silver calcium alginate antibacterial dressing after the oven dry, perhaps with 0.1～5% nanometer silver paste dipping, the method of nano silver calcium alginate dressing is made in oven dry, the raw material that this method adopts is a nanometer silver paste, in actual production, adopting directly, spraying nanometer silver paste method exists alginic acid fibre dressing easily to harden equally, the problem of process uniformity difference, and the employing infusion process, then often need to adopt the nanometer silver paste of higher concentration to implement, also have the problem of lack of homogeneity.
Summary of the invention
The objective of the invention is to overcome the deficiency that prior art exists, a kind of concentration method absorption simple substance silver particle is provided, obtain to have alginic acid fibre of good bulkiness and strong disinfecting effect and preparation method thereof.
Technical scheme of the present invention provides a kind of year silver-colored alginic acid fibre, and by weight percentage, the silver content that carries in the silver-colored alginic acid fibre is 0.01～4%.
The preparation method of a kind of as claimed in claim 1 year silver-colored alginic acid fibre comprises the steps:
(1) be 0.1～10% alkylation cyclodextrin aqueous solution with mass percent with molality be that the silver ammino solution of 0.01～1.0mol/L mixes with 1: 100～1: 10 volume ratio, stirred under 10～100 ℃ temperature conditions 1～120 minute, obtaining average grain diameter is the nano-class silver colloidal solution of 1～100nm;
(2) be the nano-silver water solution of 20～1000ug/L with the nano-class silver colloidal solution dilution that obtains for mass concentration,, alginic acid fibre impregnated in the nano-silver water solution that the impregnation process time is 2～60 minutes by bath raio 1: 10～200;
(3) the silver-colored alginic acid fibre that carries that will adsorb the simple-substance nano silvery particle takes out, and with aqueous solutions of organic solvent or organic solvent washing, obtains carrying silver-colored alginic acid fibre after the drying; Described organic solvent is a kind of in ethanol, acetone, chloroform and the isopropyl alcohol, or several compound in them.
Described aqueous solutions of organic solvent, percentage by volume, the concentration of organic solvent is 10～90%.
The method of silver-colored alginic acid fibre is carried in preparation provided by the invention, the principle of its foundation is a concentration method, promptly rely on the adsorption and enrichment characteristic of simple-substance nano silvery particle on alginic acid fibre, adopt low concentration, high bath raio simple substance silver solution-treated, obtain the method that high silver content carries silver-colored alginic acid fibre; Adopt certain density aqueous solutions of organic solvent washing and oven dry to carry silver-colored alginic acid fibre simultaneously, not only give its good bulkiness and flexibility, be convenient to the processing of later process, and can guarantee that washing process does not reduce the anti-microbial property that carries silver-colored alginic acid fibre.
Compared with prior art, advantage of the present invention is:
1, adopt the aqueous solution of the simple substance silver of big bath raio, low concentration that alginic acid fibre is carried out the concentration method impregnation process, the uniformity that helps the adsorbed nano-Ag particles in alginic acid fibre surface, help to obtain high silver content and carry silver-colored alginic acid fibre, the percentage by weight of its silver content can reach 4%, have excellent anti-microbial property, can be applicable in the disposable biological field of medical materials such as Wound dressing, hemostatic material.
2, through the silver-colored alginic acid fibre that carries of certain density aqueous solutions of organic solvent washing, oven dry, have good bulkiness and flexibility, be convenient to the processing of later process, guarantee not reduce the anti-microbial property that carries silver-colored alginic acid fibre simultaneously.
3, adopt low concentration simple substance silver solution-treated, can reduce the waste of simple substance silver solution effectively.
4, safe preparation process, process conditions are simple, and used organic solvent can reuse, and low production cost has actual application value.
The specific embodiment
Below in conjunction with embodiment technical solution of the present invention is further described.
Embodiment 1
Publication number is in the Chinese invention patent " preparation method of nano-class silver colloidal solution " of CN101837465A, a kind of technical scheme for preparing nano-class silver colloidal solution is disclosed, be 0.1%～10% alkylation cyclodextrin aqueous solution with mass percent with molality be that the silver ammino solution of 0.01～1.0mol/L mixes with 1: 100～1: 10 volume ratio, stirred under 10～100 ℃ temperature conditions 1～120 minute, obtaining average grain diameter is the nano-class silver colloidal solution of 1～100nm.
In the present embodiment, by technique scheme, be 0.5% alkylation cyclodextrin aqueous solution with mass percent with molality be that the silver ammino solution of 0.5mol/L mixes with 1: 10 volume ratio, stirred 20 minutes under 100 ℃ temperature conditions, obtaining average grain diameter is the nano-class silver colloidal solution of 1～100nm.
Above-mentioned nano-class silver colloidal solution is diluted with water to mass concentration 100ug/L, 1 kilogram of alginic acid fibre be impregnated in wherein; bath raio is 1: 50; impregnation process 10 minutes; the silver-colored alginic acid fibre that carries that again enrichment is adsorbed simple substance silver particle takes out; with 30 kilograms of concentration is the ethanol water washing back oven dry of 80% (V/V), obtains carrying silver-colored alginic acid fibre.
The preparation method of Comparative Examples: it is 100ug/L that the Nano silver solution of outsourcing is diluted to concentration with deionized water, pressed bath raio 1: 50,1 kilogram of alginic acid fibre be impregnated in wherein, handled 2 minutes, after taking out alginic acid fibre, through 30 kilograms of concentration is the ethanolic solution washing back oven dry of 80% (V/V), obtains a year silver-colored alginic acid fibre.
Compare with Comparative Examples, behind the adding alginic acid fibre, solution is become colourless gradually by original golden yellow in the 100ug/L simple-substance nano silvery solution that adopts the preparation of present embodiment technical scheme, and alginic acid fibre becomes brown gradually, and the absorption of a large amount of simple substance silver is obviously arranged; And not variable color of the alginic acid fibre in the Comparative Examples, and 100ug/L simple substance silver solution do not have any change color, shows that this method of employing do not have tangible adsorption and enrichment effect to alginic acid fibre.
With reference to EPA 3052:1996/ICP-OES, the silver-colored alginic acid fibre that carries of present embodiment and Comparative Examples preparation is carried out silver content respectively and measures, its comparing result is referring to table 1.
Table 1
As can be seen from Table 1, adopt the simple substance silver solution of present embodiment technical scheme preparation, alginic acid fibre is had strong adsorption and enrichment effect, can obtain the silver-colored alginic acid fibre that carries of higher concentration.
The nano-silver water solution that the present invention adopts, because with the alkylation cyclodextrin that contains long-chain is reductant and stabilizing agent, the alkylation cyclodextrin of this belt length chain and the big molecule of alginic acid fibre have stronger absorption affinity, thereby realized the enrichment suction-operated of simple substance silver, and feel is fluffy, soft, can be applicable to disposable biological field of medical materials such as Wound dressing, hemostatic material.
Embodiment 2
Prepare nano-silver water solution by embodiment 1 technical scheme.
1 kilogram of alginic acid fibre be impregnated in the above-mentioned nano-silver water solution that concentration is 20ug/L, pressed bath raio 1: 100, dipping place 60 minutes, the silver-colored alginic acid fibre that carries that then enrichment is adsorbed simple substance silver particle takes out, through 30 kilograms of concentration is the aqueous acetone solution washing back oven dry of 80% (V/V), obtains fluffy, the soft year silver-colored alginic acid fibre of the about 2000mg/kg of silver content.
Embodiment 3
Prepare nano-silver water solution by embodiment 1 technical scheme.
1 kilogram of alginic acid fibre be impregnated in the nano-silver water solution that concentration is 200ug/L; bath raio 1: 50; flooded 60 minutes; the silver-colored alginic acid fibre that carries that then enrichment is adsorbed the silver-colored particle of simple substance takes out; oven dry after 30 kilograms of chloroforms washings, obtain fluffy, the soft year silver-colored alginic acid fibre of the about 10000mg/kg of silver content.
Embodiment 4
Prepare nano-silver water solution by embodiment 1 technical scheme.
1 kilogram of alginic acid fibre be impregnated in the nano-silver water solution that concentration is 1000ug/L; bath raio 1: 40; flooded 60 minutes; the silver-colored alginic acid fibre that carries that then enrichment is adsorbed simple substance silver particle takes out; through 30 kilograms of concentration is the isopropanol water solution washing back oven dry of 60% (V/V), obtain fluffy, the soft year silver-colored alginic acid fibre of the about 40000mg/kg of silver content.
Claims (2)
1. a preparation method of carrying silver-colored alginic acid fibre is characterized in that comprising the steps:
(1) be 0.1%～10% alkylation cyclodextrin aqueous solution with mass percent with molality be that the silver ammino solution of 0.01～1.0mol/kg mixes with 1: 100～1: 10 volume ratio, stirred under 10～100 ℃ temperature conditions 1～120 minute, obtaining average grain diameter is the nano-class silver colloidal solution of 1～100nm;
(2) be the nano-silver water solution of 20～1000ug/L with the nano-class silver colloidal solution dilution that obtains for mass concentration,, alginic acid fibre impregnated in the nano-silver water solution that the impregnation process time is 2～60 minutes by bath raio 1: 10～200;
(3) alginic acid fibre that will adsorb the simple-substance nano silvery particle takes out, and with aqueous solutions of organic solvent or organic solvent washing, obtains carrying silver-colored alginic acid fibre after the drying, and by weight percentage, the silver content that carries in the silver-colored alginic acid fibre is 0.01～4%; Described organic solvent is a kind of in ethanol, acetone, chloroform and the isopropyl alcohol, or several compound in them.
2. the preparation method of a kind of year according to claim 1 silver-colored alginic acid fibre is characterized in that: described aqueous solutions of organic solvent, and percentage by volume, the concentration of organic solvent is 10～90%.
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| CN103225134B (en) * | 2013-05-09 | 2014-12-24 | 张家港耐尔纳米科技有限公司 | Preparation method of silver-loaded active carbon fibers |
| CN104083800B (en) * | 2014-04-30 | 2016-05-04 | 佛山市优特医疗科技有限公司 | Containing silver thiosulfate complex or silver-colored amine complex can moisture absorption containing silverware and preparation method thereof |
| CN105803806A (en) * | 2016-04-21 | 2016-07-27 | 安徽皖翎羽绒制品有限公司 | Treatment method of down feather with long-acting electromagnetic radiation shielding effect |
| CN105963755B (en) * | 2016-06-29 | 2019-04-09 | 广东泰宝医疗科技股份有限公司 | A kind of alginates sustained-release antibacterial dressing and preparation method thereof |
| CN106319929B (en) * | 2016-08-17 | 2018-07-31 | 汕头市永新织造有限公司 | A kind of preparation method of ageing-resistant silk fiber |
| CN109529093A (en) * | 2018-10-29 | 2019-03-29 | 上海工程技术大学 | A kind of alginic acid fibre and preparation method thereof for wound sterilizing hemostasis |
| CN110205800B (en) * | 2019-06-06 | 2021-10-26 | 南通大学 | Preparation method of nano zinc oxide loaded alginate fiber and prepared fiber |
| CN112891602B (en) * | 2021-01-14 | 2022-06-14 | 湖北工业大学 | Composite material for sterilization, disinfection and rapid hemostasis, preparation and application |
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| CN1935268A (en) * | 2006-10-18 | 2007-03-28 | 上海川本卫生材料有限公司 | Nano silver calcium alginate antibacterial dressing |
| KR100887768B1 (en) * | 2007-06-11 | 2009-04-17 | 나노폴리(주) | Manufactur method of wet-tissue with antimicrobial and anti-fungus function |
| CN101837465B (en) * | 2010-05-10 | 2011-11-09 | 张家港耐尔纳米科技有限公司 | Preparation method of nanometer sliver colloid solution |
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Address after: 215600 Jiangsu Zhangjiagang Economic Development Zone Overseas Students Pioneer Park Patentee after: Zhangjiagang Naier Nano Technology Co.,Ltd. Patentee after: ROOSIN MEDICAL CO., LTD. Address before: 215600 Jiangsu Zhangjiagang Economic Development Zone Overseas Students Pioneer Park Patentee before: Zhangjiagang Naier Nano Technology Co.,Ltd. Patentee before: Taizhou Rongxing Anti-adhesion Dressing Co., Ltd. |