CN1623897A - Process for preparing silicon dioxide of carrying nano silver - Google Patents
Process for preparing silicon dioxide of carrying nano silver Download PDFInfo
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- CN1623897A CN1623897A CN 200410091123 CN200410091123A CN1623897A CN 1623897 A CN1623897 A CN 1623897A CN 200410091123 CN200410091123 CN 200410091123 CN 200410091123 A CN200410091123 A CN 200410091123A CN 1623897 A CN1623897 A CN 1623897A
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Abstract
A process for preparing the SiO2 gel carrying nano-Ag includes such steps as dissolving silver nitrate in deionized water, adding the solution of surfactant and reducer to generate nano-Ag sol, adding SO2 gel, and adsorbing the nano-Ag by SO2 gel particles.
Description
Technical field
The present invention relates to the dioxide/silica gel preparation of carrying nano silver, particularly a kind of antibiotic dioxide/silica gel preparation with carrying nano silver.
Technical background
Along with the raising of people's living standard, clothing, food, lodging and transportion--basic necessities of life, daily electrical home appliance and living environment have been proposed lasting aseptic requirement, nanometer silver is as a kind of novel antibacterial material, have wide spectrum, plurality of advantages such as durable, safe, thereby Application Areas expanded constantly.Inorganic antibacterial material has vast market prospect.The composition of inorganic antiseptic mainly comprises carrier and antibiotic composition, and wherein the carrier load is held antibiotic composition, guarantees that active constituent is stable, has slow-releasing simultaneously.Antibiotic composition mainly is some metal ions, and as silver, copper, zinc etc. or Nano metal powder, mercury, cadmium, lead have antibacterial ability, but harmful; Copper, nickel, brill ion have color, will influence the attractive in appearance of product; Zinc has certain germ resistance, but its antibacterial strength only is 1/1000 of a silver ions, and silver ion antimicrobial agent occupies dominant position in inorganic antiseptic, and the commercial overwhelming majority also is a carrying silver ion inorganic antibacterial sterilant on the market.The silicon dioxide colloid of carrying nano silver is a kind of nanometer silver product of excellent property, can be used as antiseptic-germicide and is extensive use of.The silicon dioxide colloid of carrying nano silver has wide Application Areas, and as aspects such as fiber, plastics, coating, textiles, potteries, its goods such as all kinds of antibacterial fiber product, plastics, ceramic, bedclothes etc. are favored by the people.The scope of application: fields such as pottery, chemical fibre, daily necessities, plastics, tame electrical article, sports goods, medical and hygiene article, coating, water treatment, building building.
The preparation of nanometer silver is a branch of metal nano material preparation, its preparation method has multiple, as chemistry redox method, chemical deposition, vapour deposition method, electrode method, Sol-Gel method etc., wherein chemical sol method is one of important method of preparation nano material." application colloid chemistry " (Zheng Shuliang etc. write, press of East China University of Science, March in 1996 the 1st edition) introduced the silver sol preparation method for the 9th page: in alkaline medium silver salt is reduced into argent with tannin.Get the 1.7%AgNO of 2ml
3Solution is diluted with water to 100ml, adds 1% tanning solution of 1ml earlier, adds 3-4 again and drips 1%K
2CO
3Solution obtains the electronegative argent colloidal sol of reddish-brown, the tannin amount after a little while, colloidal sol becomes orange-yellow.
At present, the method for preparing nano silver colloidal sol all is to adopt reductive agent is added drop-wise in the silver nitrate solution to prepare, and the nano silver colloidal sol concentration that these methods obtain is low, and reaction is difficult to control, the colloidal sol unstable, and can't mass industrialized production.
Chinese patent CN1427041 discloses at the spherical silica particle surface by metal-salt reduction method coating nanometer silver method.This method is that silicon-dioxide is distributed in the water, silica dioxide granule size 25-2000nm; Silver nitrate aqueous solution ammoniacal liquor complexing; Mix the silicon-dioxide that two liquid obtain being adsorbed with silver ammino ion, be dispersed in after the separation and add ammoniacal liquor in the polar organic solvent again and silicon ester obtains emulsion centrifugation again, add and add the reductive agent centrifugation in the entry and obtain carrying nano silver silica dioxide granule, granular size 33-2200nm.This method complex process, the carrying nano silver silica dioxide granule that obtains is thick, distribution range is wide.
The preparation of the silicon-dioxide of carrying nano silver is first preparation nanometer silver, and the surface that the absorption property that utilizes silicon dioxide colloid then is adsorbed on silicon-dioxide with nanometer silver obtains the silicon dioxide colloid of carrying nano silver.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of silicon-dioxide of carrying nano silver, this method technology is simple, cost is low, with short production cycle, the carrying nano silver silica dioxide granule that obtains is little, size evenly.
Technical scheme of the present invention is:
A kind of preparation method of silicon-dioxide of carrying nano silver, it is characterized in that, the Silver Nitrate solid joined in the deionized water dissolve, be prepared into silver nitrate solution, the solution of tensio-active agent is joined in this solution, add reductive agent again, generate the nano silver colloidal sol of particle diameter in the 1-100 nanometer, add silicon dioxide colloid then, obtain the silicon dioxide colloid of carrying nano silver.
Being fit to tensio-active agent of the present invention can be following surfactant: anion surfactant, cats product, amphoterics and nonionogenic tenside.
Being fit to anion surfactant of the present invention can be sodium lauryl sulphate, sodium laurylsulfonate, Sodium dodecylbenzene sulfonate etc.; Cats product can be palmityl trimethyl ammonium chloride, octadecyl trimethylammonium bromide etc.; Amphoterics can be polyoxyethylene 20 sorbitan monooleate, Varion CDG-K etc.; Nonionogenic tenside can be fatty alcohol-polyoxyethylene ether such as AEO fat (primary) polyoxyethylenated alcohol, peregal and alkylphenol polyoxyethylene such as polyoxyethylene octylphenol ether etc.
Being fit to reductive agent of the present invention can be organic acid, organic amine, water and hydrazine etc., and wherein, organic acid can be xitix, citric acid etc.; Organic amine can be a Ursol D.
Being fit to silicon dioxide colloid of the present invention can be silicon sol or nano silicon dispersion liquid.
Nanometer silver median size in the silicon dioxide colloid of the carrying nano silver that the present invention is prepared is less than 100 nanometers, and the nanometer silver color can be colourless, light light yellow, yellow, deep yellow, tawny, sap green, maroon, Vandyke brown, grey, grey black etc.
The silica dioxide granule of the carrying nano silver of the present invention preparation is little, size evenly, absorption fully, and technology of the present invention is simple, cost is low, with short production cycle, can produce in enormous quantities, can be widely used in anti-biotic material.
Embodiment
The present invention will be further described below by embodiment.
Embodiment 1
Silver Nitrate solid 25.6 gram joined in 75.26 liters of deionized waters dissolve under the room temperature, be prepared into silver nitrate solution; 10% (wt%) cats product cetyl trimethylammonium bromide aqueous solution is joined in the silver nitrate solution for 560 milliliters, stir, stir then and add 1600 milliliters of 1% (wt%) aqueous ascorbic acids down, after being reacted to solution under the room temperature and all transferring nanometer silver to, add 7200 milliliters of 2600 milliliters of 30% (wt%) silicon sol solutions or 10% (wt%) nano silicon dispersion liquids, being stirred to nanometer silver fully is adsorbed onto on the silica dioxide granule, centrifugation then, concentrate and obtain tawny carrying nano silver silica suspension, filter, dry, pulverize, obtain the silicon-dioxide powdery of carrying nano silver.
Embodiment 2
Silver Nitrate solid 25.6 gram joined in 73.6 liters of deionized waters dissolve under the room temperature, be prepared into silver nitrate solution; 10% (wt%) anionic aqueous solution is joined in the silver nitrate solution for 2176 milliliters, stir, be warmed up to 90 ℃, constant temperature 2 hours, stir then and add 1600 milliliters of 1% (wt%) aqueous ascorbic acids down, after being reacted to solution and all transferring nanometer silver to, add 2600 milliliters of 30% (wt%) silicon sol solutions, being stirred to nanometer silver fully is adsorbed onto on the silica dioxide granule, cooling to 40 ℃ then is 10000 ultra-filtration membrane ultrafiltration with molecular weight cut-off, and with three concentrated solution for washing of 24 liters of deionization moisture, after the continuation ultrafiltration was 8 liters to filtrate volume, obtaining silver content was the deep yellow brown carrying nano silver silicon dioxide gel of 2 grams per liters.
Embodiment 3
Silver Nitrate solid 25.6 gram joined in 73.6 liters of deionized waters dissolve under the room temperature, be prepared into silver nitrate solution; 10% (wt%) anion surfactant sodium dodecyl sulfate aqueous solution is joined in the silver nitrate solution for 2176 milliliters, stir, be warmed up to 90 ℃, constant temperature 2 hours, stir then and add 1300 milliliters of 1% (wt%) aqueous citric acid solutions down, after being reacted to solution and all transferring nanometer silver to, add 7200 milliliters of 10% (wt%) nano silicon dispersion liquids, being stirred to nanometer silver fully is adsorbed onto on the silica dioxide granule, the standing sedimentation of lowering the temperature then, concentrate and obtain tawny carrying nano silver silica suspension, filter drying, pulverize, obtain the silicon-dioxide powdery of carrying nano silver.
Embodiment 4
Silver Nitrate solid 25.6 gram joined in 73.6 liters of deionized waters dissolve under the room temperature, be prepared into silver nitrate solution; 10% (wt%) amphoterics polyoxyethylene 20 sorbitan monooleate aqueous solution is joined in the silver nitrate solution for 2500 milliliters, stir, be warmed up to 40 ℃, constant temperature 0.5 hour, stir then and add 1600 milliliters of 1% (wt%) aqueous ascorbic acids down, after being reacted to solution and all transferring nanometer silver to, add 7200 milliliters of 10% (wt%) nano silicon dispersion liquids, being stirred to nanometer silver fully is adsorbed onto on the silica dioxide granule, the centrifugation of lowering the temperature then, drying is pulverized, and obtains the silicon-dioxide powdery of carrying nano silver.
Embodiment 5
Silver Nitrate solid 25.6 gram joined in 73.6 liters of deionized waters dissolve under the room temperature, be prepared into silver nitrate solution; 10% (wt%) amphoterics Varion CDG-K aqueous solution is joined in the silver nitrate solution for 2560 milliliters, stir, be warmed up to 45 ℃, constant temperature 0.2 hour, stir then and add 1350 milliliters of 1% (wt%) Ursol D aqueous solution down, after being reacted to solution and all transferring nanometer silver to, add 7200 milliliters of 10% (wt%) nano silicon dispersion liquids, being stirred to nanometer silver fully is adsorbed onto on the silica dioxide granule, the standing sedimentation of lowering the temperature then filters drying, pulverize, obtain the silicon-dioxide powdery of carrying nano silver.
Embodiment 6
Silver Nitrate solid 25.6 gram joined in 73.6 liters of deionized waters dissolve under the room temperature, be prepared into silver nitrate solution; 10% (wt%) nonionogenic tenside peregal, 20 aqueous solution are joined in the silver nitrate solution for 2050 milliliters, stir, be warmed up to 40 ℃, constant temperature 0.5 hour, stir then and add 1500 milliliters of 1% (wt%) aqueous citric acid solutions down, after being reacted to solution and all transferring nanometer silver to, add 7200 milliliters of 10% (wt%) nano silicon dispersion liquids, being stirred to nanometer silver fully is adsorbed onto on the silica dioxide granule, centrifugation then, drying is pulverized, and obtains the silicon-dioxide powdery of carrying nano silver.
Claims (3)
1. the preparation method of the silicon-dioxide of a carrying nano silver, it is characterized in that, the Silver Nitrate solid joined in the deionized water dissolve, be prepared into silver nitrate solution, the solution of tensio-active agent is joined in this solution, add reductive agent again, generate the nano silver colloidal sol of particle diameter in the 1-100 nanometer, add silicon dioxide colloid then, obtain the silicon dioxide colloid of carrying nano silver.
2. according to the dioxide/silica gel preparation of the described carrying nano silver of claim 1, it is characterized in that wherein said reductive agent is bad hematic acid, citric acid or Ursol D.
3. according to the dioxide/silica gel preparation of the described carrying nano silver of claim 1, it is characterized in that wherein said silicon dioxide colloid is silicon sol or nano silicon dispersion liquid.
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| CN 200410091123 CN1623897A (en) | 2004-11-19 | 2004-11-19 | Process for preparing silicon dioxide of carrying nano silver |
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| CN 200410091123 CN1623897A (en) | 2004-11-19 | 2004-11-19 | Process for preparing silicon dioxide of carrying nano silver |
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Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100376348C (en) * | 2005-10-25 | 2008-03-26 | 浙江大学 | Method for preparing nano silver on silica-gel surface |
| CN100384572C (en) * | 2005-12-29 | 2008-04-30 | 黄德欢 | Preparation method of inorganic carried nanometer silver sol |
| CN101912638A (en) * | 2010-07-26 | 2010-12-15 | 郭云童 | Nano silver-carrying-silicon dioxide catheter and production method thereof |
| CN101238817B (en) * | 2008-03-06 | 2011-09-14 | 刘燕平 | Bacteriostat, far-infrared ray emitting agent, mother particle, fiber and manufacturing method thereof |
| CN105949989A (en) * | 2016-06-20 | 2016-09-21 | 中物功能材料研究院有限公司 | Water-based UV anti-bacterial coating and preparing method thereof |
| CN106702728A (en) * | 2016-07-13 | 2017-05-24 | 东莞市恩科化工有限公司 | Ag-TIO2 composite antibacterial agent and preparation method thereof |
| CN107033426A (en) * | 2016-10-28 | 2017-08-11 | 南京财经大学 | A kind of key technology of rice anti-mildew fresh-keeping |
| CN107646885A (en) * | 2017-08-07 | 2018-02-02 | 吴杨 | A kind of sterilized eliminating smell agent and preparation method thereof |
| CN108385374A (en) * | 2018-02-12 | 2018-08-10 | 西安工程大学 | A kind of preparation method of silver-loaded silica antiseptic |
| CN109452309A (en) * | 2018-12-21 | 2019-03-12 | 三河市京纳环保技术有限公司 | A kind of preparation method of silicon substrate carrying silver antimicrobials |
| CN112898876A (en) * | 2021-03-30 | 2021-06-04 | 重庆多次元新材料科技有限公司 | High-adhesion nano-silver composite cationic epoxy resin antibacterial coating and preparation method thereof |
| CN114871426A (en) * | 2022-05-20 | 2022-08-09 | 爱科美材料科技(南通)有限公司 | Mesoporous alumina in-situ coated nano-silver material, preparation method and application |
| CN115445610A (en) * | 2022-09-23 | 2022-12-09 | 华中科技大学 | Preparation method of silver nano catalyst with high catalytic activity, product and application thereof |
| CN115592126A (en) * | 2022-10-27 | 2023-01-13 | 陕西煤业化工技术研究院有限责任公司（Cn） | Method for preparing silver powder by adopting nonmetal inducer |
| CN115676838A (en) * | 2022-10-17 | 2023-02-03 | 广东粤港澳大湾区国家纳米科技创新研究院 | Nano silicon dioxide solution and preparation method and application thereof |
-
2004
- 2004-11-19 CN CN 200410091123 patent/CN1623897A/en active Pending
Cited By (21)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100376348C (en) * | 2005-10-25 | 2008-03-26 | 浙江大学 | Method for preparing nano silver on silica-gel surface |
| CN100384572C (en) * | 2005-12-29 | 2008-04-30 | 黄德欢 | Preparation method of inorganic carried nanometer silver sol |
| CN101238817B (en) * | 2008-03-06 | 2011-09-14 | 刘燕平 | Bacteriostat, far-infrared ray emitting agent, mother particle, fiber and manufacturing method thereof |
| CN101912638A (en) * | 2010-07-26 | 2010-12-15 | 郭云童 | Nano silver-carrying-silicon dioxide catheter and production method thereof |
| CN105949989A (en) * | 2016-06-20 | 2016-09-21 | 中物功能材料研究院有限公司 | Water-based UV anti-bacterial coating and preparing method thereof |
| CN106702728A (en) * | 2016-07-13 | 2017-05-24 | 东莞市恩科化工有限公司 | Ag-TIO2 composite antibacterial agent and preparation method thereof |
| CN107033426A (en) * | 2016-10-28 | 2017-08-11 | 南京财经大学 | A kind of key technology of rice anti-mildew fresh-keeping |
| CN107646885B (en) * | 2017-08-07 | 2020-05-22 | 吴杨 | High-efficiency sterilization deodorant and preparation method thereof |
| CN107646885A (en) * | 2017-08-07 | 2018-02-02 | 吴杨 | A kind of sterilized eliminating smell agent and preparation method thereof |
| CN108385374A (en) * | 2018-02-12 | 2018-08-10 | 西安工程大学 | A kind of preparation method of silver-loaded silica antiseptic |
| CN108385374B (en) * | 2018-02-12 | 2021-01-08 | 西安工程大学 | Preparation method of silver-loaded silicon dioxide antibacterial agent |
| CN109452309A (en) * | 2018-12-21 | 2019-03-12 | 三河市京纳环保技术有限公司 | A kind of preparation method of silicon substrate carrying silver antimicrobials |
| CN112898876A (en) * | 2021-03-30 | 2021-06-04 | 重庆多次元新材料科技有限公司 | High-adhesion nano-silver composite cationic epoxy resin antibacterial coating and preparation method thereof |
| CN114871426B (en) * | 2022-05-20 | 2023-12-22 | 爱科美材料科技(南通)有限公司 | Mesoporous alumina in-situ coated nano silver material, preparation method and application |
| CN114871426A (en) * | 2022-05-20 | 2022-08-09 | 爱科美材料科技(南通)有限公司 | Mesoporous alumina in-situ coated nano-silver material, preparation method and application |
| CN115445610A (en) * | 2022-09-23 | 2022-12-09 | 华中科技大学 | Preparation method of silver nano catalyst with high catalytic activity, product and application thereof |
| CN115445610B (en) * | 2022-09-23 | 2024-05-14 | 华中科技大学 | Preparation method of silver nano catalyst with high catalytic activity, product and application thereof |
| CN115676838A (en) * | 2022-10-17 | 2023-02-03 | 广东粤港澳大湾区国家纳米科技创新研究院 | Nano silicon dioxide solution and preparation method and application thereof |
| CN115676838B (en) * | 2022-10-17 | 2024-05-03 | 广东粤港澳大湾区国家纳米科技创新研究院 | Nano silicon dioxide solution and preparation method and application thereof |
| CN115592126A (en) * | 2022-10-27 | 2023-01-13 | 陕西煤业化工技术研究院有限责任公司（Cn） | Method for preparing silver powder by adopting nonmetal inducer |
| CN115592126B (en) * | 2022-10-27 | 2024-01-30 | 陕西煤业化工技术研究院有限责任公司 | Method for preparing silver powder by adopting nonmetallic inducer |
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