CN103202317A - Silver iodine complexing antibacterial agent and preparation method thereof - Google Patents
Silver iodine complexing antibacterial agent and preparation method thereof Download PDFInfo
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- CN103202317A CN103202317A CN2013101318892A CN201310131889A CN103202317A CN 103202317 A CN103202317 A CN 103202317A CN 2013101318892 A CN2013101318892 A CN 2013101318892A CN 201310131889 A CN201310131889 A CN 201310131889A CN 103202317 A CN103202317 A CN 103202317A
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Abstract
The invention discloses a silver iodine complexing antibacterial agent and a preparation method thereof. The preparation method comprises the following steps of: preparing an iodate aqueous solution and a silver salt aqueous solution, the molar concentrations of which are respectively 0.01-1.0mol/L, controlling flow rate under the conditions of stirring and at the temperature of 20-90 DEG C, injecting the matters into a macromolecule complexing agent aqueous solution, generating the silver iodine in site in the macromolecule complexing agent, and then carrying out ultrasound treatment for 30-60 minutes under the condition of reaction temperature to obtain a silver iodine complex dispersion liquid. According to the preparation method, the nanometer silver iodine is generated in site in the macromolecule complexing agent by using the inhibition effect of the macromolecule complexing agent, and the prepared silver iodine has small particle size, is narrow in distribution and is easy to stably disperse in water. The silver iodine complexing antibacterial agent provided by the invention has the sterilizing rate up to 99.9% and can be added to other materials, so that the antibacterial property of the materials is improved; and the silver iodine complexing antibacterial agent can be used for disinfection and sterilization of the surfaces of skins, medical apparatus and instruments, household ware and the like.
Description
Technical field
The present invention relates to a kind of silver iodide complexing antibacterial agent and preparation method, belong to the function nano field of material preparation.
Background technology
In recent years, raising along with progress of science and technology and living standards of the people, people's health care consciousness and awareness of safety strengthen day by day, the disease that causes owing to harmful microorganism in the environment is more and more general, so active development is various becomes researcher's research focus with people's closely-related anti-biotic material of living.
The research of anti-biotic material also will be considered the convenience of itself safety, production cost and use when considering antibacterial effect itself.In general antibacterial agent is divided into natural antibacterial agent, organic antibacterial agent and inorganic antiseptic three major types.
Natural antibacterial agent mainly contains some extract from natural plants, animal, insect and microorganism, and its advantage is pollution-free, good biocompatibility, but antibacterial functions is limited, and difficulty has long-acting broad-spectrum antibacterial, non-refractory, not wash resistant.
Organic antibacterial agent mainly is quaternary ammonium salt, phenol, ureas and guanidine class, heterocyclic and organo-metallic compound, initial sterilizing power is strong, sterilization is namely imitated and broad-spectrum antibacterial property is good, price is relatively cheap, but poor chemical stability, thermo-labile, non-refractory, secondary product are often poisonous, easily move during use, the antibiotic life-span is short.
Inorganic antiseptic is 20th century antibacterial agents just succeeded in developing of the mid-80, also is the focus of present antibacterial agent research, has represented the developing direction of antibacterial agent.Mainly divide three classes at present: a class is mineral salt or the complex compound of metal ion; Second class is that zinc oxide, titanium oxide are photocatalysis (photocatalyst) antibacterial agent of representative; The 3rd class is Nano Silver simple substance antibacterial agent.
First kind inorganic antiseptic antibacterial mechanisms is positively charged metal ion and electronegative cell membrane generation Coulomb attraction, the metal ion permeates cell membranes enters in the bacterium and the sulfonium base on the bacterial body internal protein, amino react, destroy the activity of the cell synzyme of bacterium, make cell forfeiture schizogamy ability and death.This class antibacterial agent safety is good, but poor stability, easily variable color, and be generally powder, need before the use to disperse.
The second class inorganic antiseptic antibacterial mechanisms is to produce electron hole pair under state is penetrated in illumination; activate the oxygen in air or the water; produce hydroxyl radical free radical and active oxygen anion (O2-); these two kinds of free radicals are all very active; the cell of directtissima bacterium when running into bacterium; extract organic H atom or attack its unsaturated bond, cause bacterioprotein variation and lipolysis.But this class antibacterial agent needs the irradiation of ultraviolet light, also needs before the use to disperse again.
From safety and antibacterial effect, the 3rd class inorganic antiseptic Nano Silver simple substance antibacterial agent is more promising, but silver changes brown silver oxide easily into or is reduced into the simple substance silver of black, and the cost height, will solve core and two big difficult points that discoloration problem and the problem of reducing cost are considered as the inorganic antiseptic technology of preparing in the world all the time.Chinese invention patent CN1586774A discloses a kind of preparation method of nano-class silver colloidal solution, this method adopts double injecting control technology, injecting silver-colored ammonia spirit and the reductant aqueous solution in addition simultaneously, the aqueous solution of reductant obtains product, this method equipment cost height, the pH value is high after using ammoniacal liquor, sharp aroma is arranged, and application is restricted, and unreacted silver ion is seen phototropic.Chinese invention patent CN1583332A discloses a kind of preparation method of nano-class silver colloidal solution; using under the condition of disperseing protecting colloid and reductant; obtain the less Nano Silver of granularity; this technology exists unreacted silver ion to see the shortcoming of phototropic equally; and disperse instability, use restricted.Chinese invention patent CN 1673093A discloses a kind of preparation method of nanoscale silver iodide powder, it is slowly to be added drop-wise in the potassium iodide clear aqueous solution that contains dispersant under normal temperature, atmospheric pressure state and fully stirring simultaneously with containing silver nitrate, complexing agent, obtain the following nano silver iodide precipitation of 100nm behind the standing sedimentation, this silver iodide sediment is through filtering, washing, drying, just obtaining granularity is nano silver iodide powder.
Common silver iodide are because there is photosensitivity, and the catalyzer in only being used as developer and increasing rain artificially for a long time also is used for medical industry sometimes.Because the lability of silver iodide, oral, local contact or occupational contact this product for a long time, can cause the silver calmness of part or general, part or whole skin hemachromatosis, eye infringement, chronic bronchitis etc. take place, therefore silver iodide do not use as antibacterial agent up to now.
Summary of the invention
The objective of the invention is to overcome the deficiency that prior art exists, a kind of cheap, easy to use, antibacterial agent of silver iodide complexing safely and effectively and preparation method thereof is provided.
Realize that the technical scheme of the object of the invention provides a kind of preparation method of silver iodide complexing antibacterial agent, comprises the steps:
1, a kind of in polyvinylpyrrolidone, carboxymethyl cellulose, hydroxyethylcellulose, polycarboxylic acids, the poly or their any combination are dissolved in the water, compound concentration is 0.1～2.0g/L polymeric complexing agent aqueous solution;
2, prepare iodine salt water solution and the silver salt solution that molar concentration is 0.01～1.0mol/L respectively, stirring and temperature is under 20～90 ℃ the condition, iodine salt water solution and silver salt solution are injected in the polymeric complexing agent aqueous solution, iodine salt water solution and silver salt solution and polymeric complexing agent aqueous solution volume ratio are controlled respectively in 1:10～50, inject flow-control at 0.15～0.50ml/s, original position generates silver iodide in polymeric complexing agent;
3, be ultrasonic processing 30～60min under 20～90 ℃ the condition in temperature, obtain a kind of silver iodide complexing antibacterial agent.
The technical scheme of optimization of the present invention is: described silver salt is one or both the combination in silver nitrate, the silver sulfate.Described salt compounded of iodine is one or both the combination in potassium iodide, the sodium iodide.To be injected into the injection mode in the polymeric complexing agent aqueous solution be single titration, two titration or spraying method for iodine salt water solution and silver salt solution in the step 2.
Technical solution of the present invention also comprises a kind of silver iodide complexing antibacterial agent that obtains by above-mentioned preparation method.
Principle of the present invention is: be carrier with the polymeric complexing agent that has no side effect, by the synthetic silver iodide nano material of original position synthetic technology original position on polymeric complexing agent, obtain silver iodide complexing dispersion, utilize the good physiology inertia of polymeric complexing agent, and good biocompatibility, silver iodide and polymeric complexing agent that technical solution of the present invention obtains have synergistic effect, and skin, mucous membrane, eye etc. are not formed any stimulation, have overcome the deficiency that existing silver-series antibacterial agent exists.It also has stronger antibacterial action and excellent dispersion properties, and can be added on to use in the other materials increases the material anti-microbial property, also can be directly used in the surface sterilization sterilization of skin, medicine equipment, household wares.
Compared with prior art, outstanding advantage of the present invention is:
1, the present invention utilizes the synergy of nano silver iodide and polymeric complexing agent to realize antibacterial effect, no metachromatism, and cost is low, is different from existing simple substance silver antibacterial agent and silver ion antimicrobial agent product.
2, the product colorless and odorless for preparing of the present invention, pH value are neutral, and skin is not had any spread effect, have good safety, the feature of environmental protection, convenience.
3, the product stability that provides is good, and place the long period and also do not have precipitation, and convenient the use.
Description of drawings
Fig. 1 is the transmission electron microscope picture of nano particle in the prepared antibacterial agent of the embodiment of the invention 1.
Fig. 2 is the laser particle size analysis figure of nano particle in the prepared antibacterial agent of the embodiment of the invention 1.
Fig. 3 is the bacteriostasis rate result of the test figure of the prepared antibacterial agent of the embodiment of the invention 1.
Embodiment
Below by embodiment also by reference to the accompanying drawings, technical scheme of the present invention is further elaborated.
Embodiment 1:
Prepare potassium iodide aqueous solution and silver nitrate aqueous solution that molar concentration is 0.01mol/L respectively, under stirring state, be under 35 ℃ the condition in temperature, under the flow of 0.25ml/s, adopt the mode of two titration, the above-mentioned aqueous solution is injected into the good 0.05mol/L polyvinylpyrrolidone aqueous solution of configured in advance, the volume ratio of potassium iodide aqueous solution and silver nitrate aqueous solution and the polyvinylpyrrolidone aqueous solution is among the 1:20, high-speed stirred 60min, ultrasonic processing 30min under the reaction temperature condition again after finishing obtains flaxen translucent silver iodide complexing dispersion liquid.
Referring to accompanying drawing 1, by the sem photograph of nano particle in the antibacterial agent as can be known, be between 1～5nm by the granularity of nano material in the embodiment 1 described method gained antibacterial agent, be the high degree of dispersion state, particulate is evenly to exist with the single particle form basically.
Referring to accompanying drawing 2, by the laser particle size analysis figure of nano particle in the antibacterial agent as can be known, the narrow diameter distribution of nano material has only a peak in the antibacterial agent that makes by embodiment 1 described method, and average aggregate particle size is 27.81nm;
The silver iodide complexing dispersion liquid that present embodiment is provided carries out the bacteriostasis rate test, referring to accompanying drawing 3, Fig. 3 is that silver iodide complexing dispersion liquid is to colibacillary bacteriostasis rate result, by the bacteriostasis rate of nano particle in the antibacterial agent among the figure as can be known, the antibacterial agent that makes by embodiment 1 described method has stronger antibacterial characteristics.
Embodiment 2:
Prepare potassium iodide aqueous solution and the silver sulfate aqueous solution that molar concentration is 0.05mol/L respectively, under stirring state, be under 35 ℃ the condition in temperature, under the flow of 0.15ml/s, adopt the mode of spray, the above-mentioned aqueous solution is injected in the good 0.10mol/L carboxymethyl cellulose aqueous solution of configured in advance, the volume ratio of potassium iodide aqueous solution and the silver sulfate aqueous solution and carboxymethyl cellulose aqueous solution is 1:50, high-speed stirred 60min, ultrasonic processing 30min under the reaction temperature condition again after finishing obtains flaxen translucent silver iodide complexing dispersion liquid.
Embodiment 3:
Prepare sodium iodide aqueous solution and the silver sulfate aqueous solution that molar concentration is 0.05mol/L respectively, under stirring state, be under 35 ℃ the condition in temperature, under the flow of 0.15ml/s, adopt the mode of single titration, the above-mentioned aqueous solution is injected in the good 0.10mol/L hydroxyethyl cellulose aqueous solution of configured in advance, high-speed stirred 30min, ultrasonic processing 30min under the reaction temperature condition again after finishing obtains flaxen translucent silver iodide complexing dispersion liquid.
Claims (5)
1. the preparation method of a silver iodide complexing antibacterial agent is characterized in that comprising the steps:
(1) a kind of in polyvinylpyrrolidone, carboxymethyl cellulose, hydroxyethylcellulose, polycarboxylic acids, the poly or their any combination are dissolved in the water, compound concentration is 0.1～2.0g/L polymeric complexing agent aqueous solution;
(2) prepare iodine salt water solution and the silver salt solution that molar concentration is 0.01～1.0mol/L respectively, stirring and temperature is under 20～90 ℃ the condition, iodine salt water solution and silver salt solution are injected in the polymeric complexing agent aqueous solution, iodine salt water solution and silver salt solution and polymeric complexing agent aqueous solution volume ratio are controlled respectively in 1:10～50, inject flow-control at 0.15～0.50ml/s, original position generates silver iodide in polymeric complexing agent;
(3) be ultrasonic processing 30～60min under 20～90 ℃ the condition in temperature, obtain a kind of silver iodide complexing antibacterial agent.
2. the preparation method of a kind of silver iodide complexing antibacterial agent according to claim 1 is characterized in that: described silver salt is one or both the combination in silver nitrate, the silver sulfate.
3. the preparation method of a kind of silver iodide complexing antibacterial agent according to claim 1 is characterized in that: described salt compounded of iodine is one or both the combination in potassium iodide, the sodium iodide.
4. the preparation method of a kind of silver iodide complexing antibacterial agent according to claim 1 is characterized in that: the injection mode that iodine salt water solution and silver salt solution are injected in the polymeric complexing agent aqueous solution in the step (2) is single titration, two titration or spraying method.
5. silver iodide complexing antibacterial agent that obtains by claim 1 preparation method.
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| CN2013101318892A CN103202317A (en) | 2013-04-16 | 2013-04-16 | Silver iodine complexing antibacterial agent and preparation method thereof |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103843823A (en) * | 2013-12-27 | 2014-06-11 | 山东光大科技发展有限公司 | Preparation method for cellulose ether nano-silver antibacterial agent |
| CN105724430A (en) * | 2015-12-24 | 2016-07-06 | 江苏纳盾科技有限公司 | Mosquito repellent agent, and preparation and application methods thereof |
| CN106879629A (en) * | 2017-04-05 | 2017-06-23 | 南京新化原纳米科技有限公司 | A kind of multi-effective active iodine antibiotic bactericide and preparation method thereof |
| EP3103460A4 (en) * | 2014-02-07 | 2017-08-16 | NBC Meshtec, Inc. | Bactericidal composition for bacterial skin disease |
| CN109112838A (en) * | 2018-06-07 | 2019-01-01 | 苏州东展羽绒服饰有限公司 | A kind of preparation method of antibacterial deodorizing nano water-proof natural feather |
| CN111358807A (en) * | 2020-04-01 | 2020-07-03 | 赵莹 | Nano-silver modified complex iodine composite dry powder disinfection aerosol and preparation method thereof |
| CN114195480A (en) * | 2021-12-23 | 2022-03-18 | 新明珠集团股份有限公司 | Fine stain-resistant antibacterial brick and preparation method thereof |
| CN115517249A (en) * | 2022-09-23 | 2022-12-27 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of high-temperature-resistant iodine-doped mesoporous carbon nitride-loaded nano-silver efficient antibacterial agent |
| CN118058298A (en) * | 2024-04-19 | 2024-05-24 | 四川大学华西医院 | Iodine-containing cleaning disinfectant for flushing endoscope lens in operation process and preparation method thereof |
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| WO2006026026A2 (en) * | 2004-07-30 | 2006-03-09 | Acrymed, Inc. | Antimicrobial silver compositions |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103843823A (en) * | 2013-12-27 | 2014-06-11 | 山东光大科技发展有限公司 | Preparation method for cellulose ether nano-silver antibacterial agent |
| EP3103460A4 (en) * | 2014-02-07 | 2017-08-16 | NBC Meshtec, Inc. | Bactericidal composition for bacterial skin disease |
| CN105724430A (en) * | 2015-12-24 | 2016-07-06 | 江苏纳盾科技有限公司 | Mosquito repellent agent, and preparation and application methods thereof |
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| CN106879629A (en) * | 2017-04-05 | 2017-06-23 | 南京新化原纳米科技有限公司 | A kind of multi-effective active iodine antibiotic bactericide and preparation method thereof |
| CN109112838A (en) * | 2018-06-07 | 2019-01-01 | 苏州东展羽绒服饰有限公司 | A kind of preparation method of antibacterial deodorizing nano water-proof natural feather |
| CN111358807A (en) * | 2020-04-01 | 2020-07-03 | 赵莹 | Nano-silver modified complex iodine composite dry powder disinfection aerosol and preparation method thereof |
| CN114195480A (en) * | 2021-12-23 | 2022-03-18 | 新明珠集团股份有限公司 | Fine stain-resistant antibacterial brick and preparation method thereof |
| CN115517249A (en) * | 2022-09-23 | 2022-12-27 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of high-temperature-resistant iodine-doped mesoporous carbon nitride-loaded nano-silver efficient antibacterial agent |
| CN118058298A (en) * | 2024-04-19 | 2024-05-24 | 四川大学华西医院 | Iodine-containing cleaning disinfectant for flushing endoscope lens in operation process and preparation method thereof |
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Application publication date: 20130717 |