CN102198511B - Preparation method of carboxymethyl curdlan polysaccharide-based colloidal aqueous solution containing nano silver particles - Google Patents
Preparation method of carboxymethyl curdlan polysaccharide-based colloidal aqueous solution containing nano silver particles Download PDFInfo
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- CN102198511B CN102198511B CN 201110107865 CN201110107865A CN102198511B CN 102198511 B CN102198511 B CN 102198511B CN 201110107865 CN201110107865 CN 201110107865 CN 201110107865 A CN201110107865 A CN 201110107865A CN 102198511 B CN102198511 B CN 102198511B
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Abstract
The invention discloses a preparation method of carboxymethyl curdlan polysaccharide-based colloidal aqueous solution containing nano silver particles in the technical field of biomedicine. The method is implemented by the following technical scheme that: the method comprises the following steps of: mixing aqueous solution of silver nitrate and aqueous solution of carboxymethyl curdlan, wherein the concentration of the silver nitrate is 0.001 to 0.01mol/L, and the concentration of the carboxymethyl curdlan is 0.001 to 0.1g/mL; and performing ultraviolet irradiation to obtain nano silver-containing colloidal aqueous solution with different particle diameter and particle diameter distribution. The process of the method is simple; the raw materials involved in the reaction are environment-friendly and pollution-free, have biocompatibility, and do not need post treatment; and by changing the concentration of the silver nitrate, the concentration of the carboxymethyl curdlan, the molecular weight and the illumination time, the particle diameter and the particle diameter distribution of the nano silver particles are adjusted and controlled, namely the size is adjustable.
Description
Technical field
That the present invention relates to is material and the preparation method in a kind of biological medicine technology field, specifically a kind of colloid aqueous solution preparation method who contains nano-Ag particles based on the carboxymethyl curdlan gum polysaccharide.
Background technology
Argent has anti-mattress and anti-mattress wide spectrum, the bacteriums such as Escherichia coli, Pseudomonas aeruginosa, staphylococcus aureus all there is obvious sterilizing function, and the silver-colored particle of nanoscale is because its quantum size effect, surface-interface effect and macro quanta tunnel effect demonstrate again the character of the aspects such as good optics, electricity, calorifics, magnetics and chemistry, therefore have a wide range of applications at aspects such as catalysis, photoelectric device, SERS (SERS), biology sensor, biomedicines.
The preparation method of Nano Silver mainly contains chemical method and physical method both at home and abroad at present.Chemical method comprises liquid phase chemical reduction method, photoreduction method, electrochemical process, microemulsion etc.; Physical method comprises microwave irradiation, mechanical milling method, vacuum sputtering, laser burn etc.But the physical method such as vacuum sputtering, laser burn is high to equipment requirement, and energy consumption is higher; The microemulsion method complex process, need the operations such as centrifugation post processing; The liquid phase chemical reduction method is because the method that its operation relatively simply is the most normal employing.The liquid phase chemical reduction method is usually take the compound of argentiferous as raw material, under the condition that organic protective agent or dispersant exist, reduces with reducing agent.But its reducing agent commonly used such as hydrazine hydrate, sodium borohydride, formaldehyde, dimethyl formamide etc. have toxicity, and be big for environment pollution.Such as patent CN101121204A, disclosed Nano Silver preparation method relates to a large amount of uses of the organic solvents such as environmentally harmful reducing agent hydrazine hydrate and cyclohexane among CN101215450A and the CN1759962A.Patent CN101586309A, CN1653907A and CN1653907A then relate to the use of the aldehyde compounds such as formaldehyde, acetaldehyde and sodium borohydride.
At present, along with the proposition of the concept of " Green Chemistry ", Environment close friend's chemical reagent synthesizes Nano silver grain becomes inexorable trend.[the Poovathinthodiyil Raveendran such as Raveendran, Jie Fu, and Scott L.Walle n.Completely " Green " Synthesis and Stabilization of Metal Nanoparticles (the synthetic and stability of the green of metal nanoparticle) .J.AM.CHEM.SOC.2003,125,13,940 13941] proposing to adopt the starch of solubility is protective agent, β-D-Glucose is reducing agent, adds the green synthesis method of hot preparation Nano silver grain in the aqueous solution under 40 ℃; [the Junhui He such as He, Toyoki Kunitake, Aiko Nakao.Facile in Situ Synthesis of Noble Metal Nanoparticles in Porous Cellulose Fibers (utilizing the porous fibre original position to prepare noble metal nano particles) .Chem.Mater.2003,15,4401-4406] utilize the cellulose of porous to synthesize Ag for the template original position, Au, the nano particle of Pt and Pd; [the Xiaoqiang Cui such as Cui, Chang Ming Li, Haifeng Bao, Xinting Zheng, Jianfeng Zang, Chui Ping Ooi, Jun Guo.Hyaluronan-Assisted Photoreduction Synthesis of Silver Nanostructures:From Nanoparticle to Nanoplate (photo-reduction prepares nano silver particles in the presence of hyaluronic acid: nanosphere is to the transformation of nano-plates) .J.Phys.Chem.C 2008,112,10730-10734] reported under ultraviolet lighting, use hyaluronic acid to prepare the method for different-shape nano silver as stabilizing agent and reducing agent; [the Ivan Donati such as Donati, Andrea Travan, Chiara Pelillo, Tommaso Scarpa, Anna Coslovi, Alois Bonifacio, Valter Sergo, and Sergio Paoletti.Polyol Synthesis of Silver Nanoparticles:Mechanism of Reduction by Alditol Bearing Polysaccharides.Biomacromolecules (utilizes the polyol synthesizing nano-silver: the reduction mechanism of polysaccharide) 2009,10,210-213] adopt chitosan derivatives to prepare nano-Ag particles as reducing agent and stabilizing agent.Also relevant for the green synthesis method that adopts the polysaccharide large biological molecule as protective agent and reducing agent, CN101407586A discloses a kind of nano silver/dextran gel hybridization material and preparation method thereof such as patent in the patent aspect.The method is at first glucan to be prepared into gel, prepares nano silver/dextran gel hybridization material by glucan in-situ reducing silver ion; Adopt carboxymethyl cellulose as reducing agent and protective agent among the patent CN101450385A, at 80 ℃ of lower preparation nano silver colloid aqueous solutions.The polysaccharide large biological molecule has hydrophily, biocompatibility, degradability, particularly has polyhydroxy functional groups, possesses reduction characteristic, can play the effect of reducing nano-silver under the condition of not adding other poisonous reducing agents.
Carboxymethyl curdlan gum is as a kind of Curdlan polysaccharide derivates of polyanion, has good immunocompetence [Y Ohya et al.Immunological enhancement activityof muramyl dipeptide analogue/CM-curdlan conjugate.Carbohydrate polymers.1994,23,47-54; X Bao et al., Chemical modifications of the (1-3)-β-D-glucan from spores of Ganoderma lucidum and investigation of their physicochemical properties and immunological activity (immune-enhancing activity of muramyl dipeptide analog/carboxymethyl curdlan gum complex compound; Derive from chemical modification and physical and chemical performance and the immunocompetent research of (the 1-3)-callose of glossy ganoderma gemma) .Carbohydrate Research.2001,336,127-140], make the nano silver colloid aqueous solution that makes in biological medicine, the fields such as anti-mattress have widely uses.And Curdlan (curdlan) is a kind of straight chain type 1 of microbial fermentation, the 3-callose, itself has obtained the approval of U.S. FDA (Food and Drug Admistraton) in 1996, can be used as food additives and be applied to [Cong Fengsong in the food, Zhang Weijie, Zhang Hongbin. Curdlan and on food and medicine application, Food Science, 2004,11:432-435].Therefore, because the biocompatibility that possesses of carboxymethyl curdlan gum, adopt it to prepare Nano Silver as reducing agent and stabilizing agent and have larger advantage.
Summary of the invention
The present invention is directed to the prior art above shortcomings; a kind of colloid aqueous solution preparation method who contains nano-Ag particles based on the carboxymethyl curdlan gum polysaccharide is provided; use silver nitrate as raw material; water is as solvent; carboxymethyl curdlan gum is as protective agent and reducing agent; prepare nano silver colloid aqueous solution under the condition of ultraviolet lighting, the concentration that prepared nano-Ag particles size can be by changing silver nitrate, the concentration of carboxymethyl curdlan gum and molecular weight and light application time are regulated and control.This preparation method's process is simple, related raw material environmental friendliness in the reaction, pollution-free, have biocompatibility, need not post processing, and prepared dispersed nano-silver particles and having good stability.
The present invention is achieved through the following technical solutions, the present invention by with silver nitrate aqueous solution and carboxymethyl curdlan gum aqueous solution and wherein the concentration of silver nitrate be 0.001-0.01mol/L, the concentration of carboxymethyl curdlan gum is 0.001-0.1g/mL, through obtaining containing the nano silver colloid aqueous solution of different-grain diameter and particle diameter distribution behind the ultraviolet irradiation.
The concentration of described silver nitrate aqueous solution is 0.01-0.1mol/L;
The concentration of the described carboxymethyl curdlan gum aqueous solution is 0.01-1g/mL;
The molecular weight of described carboxymethyl curdlan gum is 90,000-800,000.
Described mixing refers to: control pH scope was 6～8 and adopts under the lucifuge environment and stir after described two kinds of solution were mixed.
Described ultraviolet irradiation refers to: illumination 1-24h under the uviol lamp of employing wavelength X=365nm.
The present invention has abandoned the heating steps in traditional liquid phase chemical reduction method, adopts the low-power uviol lamp to carry out light radiation, has avoided polymer degradation that high-temperature heating causes and the inequality of being heated of solution; Use to adopt the dispersed nano-silver particles of the present invention's preparation and have good stability, and the concentration of concentration that can be by changing silver nitrate, carboxymethyl curdlan gum and molecular weight and light application time distribute to nano-Ag particles particle diameter and particle diameter; The carboxymethyl curdlan gum polysaccharide macro-molecular is as reducing agent and stabilizing agent, one-step method can obtain required nano silver colloid aqueous solution, and have certain biocompatibility, product need not further separation and purification treatment, can directly apply to the technical fields such as biological medicine, sterilization; Simultaneously, preparation is simple, reaction condition is gentle, easily control; Because Nano Silver is the bactericide of wide spectrum, and fungus and bacterium is all had preferably inhibitory action, the prepared nano silver colloid aqueous solution of the present invention can be concentrated by rotary evaporation, and casting film-forming is made the anti-mattress film of Nano Silver/carboxymethyl curdlan gum.
Description of drawings
The nano-Ag particles transmission electron microscope schematic diagram of Fig. 1 embodiment 1.
The X ray diffracting spectrum of the nano-Ag particles of Fig. 2 embodiment 1.
The nano-Ag particles transmission electron microscope schematic diagram of Fig. 3 embodiment 2.
The nano-Ag particles transmission electron microscope schematic diagram of Fig. 4 embodiment 4.
The nano-Ag particles transmission electron microscope schematic diagram of Fig. 5 embodiment 5.
The nano-Ag particles transmission electron microscope schematic diagram of Fig. 6 embodiment 6.
The nano-Ag particles transmission electron microscope schematic diagram of Fig. 7 embodiment 9.
The specific embodiment
The below elaborates to embodiments of the invention, and present embodiment is implemented under take technical solution of the present invention as prerequisite, provided detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following embodiment.
The 0.43g silver nitrate is dissolved in deionized water, and constant volume is in the brown volumetric flask of 50mL, and preparation concentration is the 0.05mol/L silver nitrate aqueous solution; With 0.02g carboxymethyl curdlan gum (M
w≈ 800,000) be dissolved in the 20mL deionized water, preparation concentration is the carboxymethyl curdlan gum aqueous solution of 0.1g/mL; With 0.2mL silver nitrate aqueous solution and 0.5mL carboxymethyl curdlan gum aqueous solution, adding deionized water, to make overall solution volume be 5mL again, wherein the concentration of silver nitrate is 0.002mol/L, the concentration of carboxymethyl curdlan gum is 0.01g/mL, controlling its pH scope is 6～8, the dark place lucifuge mixes under the room temperature, solution being placed wavelength is illumination 24h under the 365nm uviol lamp again, obtain the Yellow nanometer silver colloid aqueous solution, transmission electron microscope results as shown in Figure 1, the particle diameter of the nano-Ag particles that obtains on average is about 10nm, its X ray diffracting spectrum such as Fig. 2.
The 0.43g silver nitrate is dissolved in deionized water, and constant volume is in the brown volumetric flask of 50mL, and preparation concentration is the 0.05mol/L silver nitrate aqueous solution; With 0.02g carboxymethyl curdlan gum (M
w≈ 800,000) be dissolved in the 20mL deionized water, preparation concentration is the carboxymethyl curdlan gum aqueous solution of 0.1g/mL; With 0.2mL silver nitrate aqueous solution and 0.5mL carboxymethyl curdlan gum aqueous solution, adding deionized water, to make overall solution volume be 5mL again, wherein the concentration of silver nitrate is 0.002mol/L, the concentration of carboxymethyl curdlan gum is 0.01g/mL, controlling its pH scope is 6～8, the dark place lucifuge mixes under the room temperature, solution being placed wavelength is illumination 1h under the 365nm uviol lamp again, obtain the lightpink nano silver colloid aqueous solution, transmission electron microscope results as shown in Figure 3, prepared nano-Ag particles particle diameter distributes wide, and size is from 5nm to 60nm.
Embodiment 3
The 0.43g silver nitrate is dissolved in deionized water, and constant volume is in the brown volumetric flask of 50mL, and preparation concentration is the 0.05mol/L silver nitrate aqueous solution; With 0.02g carboxymethyl curdlan gum (M
w≈ 800,000) be dissolved in the 20mL deionized water, preparation concentration is the carboxymethyl curdlan gum aqueous solution of 0.1g/mL; With 0.2mL silver nitrate aqueous solution and 0.5mL carboxymethyl curdlan gum aqueous solution, adding deionized water, to make overall solution volume be 5mL again, wherein the concentration of silver nitrate is 0.002mol/L, the concentration of carboxymethyl curdlan gum is 0.01g/mL, controlling its pH scope is 6～8, the dark place lucifuge mixes under the room temperature, solution being placed wavelength is illumination 7h under the 365nm uviol lamp again, obtain faint yellow nano silver colloid aqueous solution, the nano particle diameter narrowly distributing that the particle diameter of prepared nano-Ag particles distributes and makes than illumination 1h, size is from 5nm to 30nm.
Embodiment 4
The 0.43g silver nitrate is dissolved in deionized water, and constant volume is in the brown volumetric flask of 50mL, and preparation concentration is the 0.05mol/L silver nitrate aqueous solution; With 0.02g carboxymethyl curdlan gum (M
w≈ 90,000) be dissolved in the 20mL deionized water, preparation concentration is the carboxymethyl curdlan gum aqueous solution of 0.1g/mL; With 0.2mL silver nitrate aqueous solution and 0.5mL carboxymethyl curdlan gum aqueous solution, adding deionized water, to make overall solution volume be 5mL again, wherein the concentration of silver nitrate is 0.002mol/L, the concentration of carboxymethyl curdlan gum is 0.01g/mL, controlling its pH scope is 6～8, the dark place lucifuge mixes under the room temperature, solution being placed wavelength is illumination 24h under the 365nm uviol lamp again, obtain light yellow nano silver colloid aqueous solution, transmission electron microscope results as shown in Figure 4, the particle diameter of the nano-Ag particles that obtains on average is about 100nm.
Embodiment 5
The 0.43g silver nitrate is dissolved in deionized water, and constant volume is in the brown volumetric flask of 50mL, and preparation concentration is the 0.05mol/L silver nitrate aqueous solution; With 0.02g carboxymethyl curdlan gum (M
w≈ 450,000) be dissolved in the 20mL deionized water, preparation concentration is the carboxymethyl curdlan gum aqueous solution of 0.1g/mL; With 0.2mL silver nitrate aqueous solution and 0.5mL carboxymethyl curdlan gum aqueous solution, adding deionized water, to make overall solution volume be 5mL again, wherein the concentration of silver nitrate is 0.002mol/L, the concentration of carboxymethyl curdlan gum is 0.01g/mL, controlling its pH scope is 6～8, the dark place lucifuge mixes under the room temperature, solution being placed wavelength is illumination 24h under the 365nm uviol lamp again, obtain the Yellow nanometer silver colloid aqueous solution, transmission electron microscope results as shown in Figure 5, the particle diameter of the nano-Ag particles that obtains on average is about 50nm.
Embodiment 6
The 0.085g silver nitrate is dissolved in deionized water, and constant volume is in the brown volumetric flask of 50mL, and preparation concentration is the 0.01mol/L silver nitrate aqueous solution; With 0.02g carboxymethyl curdlan gum (M
w≈ 800,000) be dissolved in the 2mL deionized water, preparation concentration is the carboxymethyl curdlan gum aqueous solution of 0.01g/mL; With 0.5mL silver nitrate aqueous solution and 0.5mL carboxymethyl curdlan gum aqueous solution, adding deionized water, to make overall solution volume be 5mL again, wherein the concentration of silver nitrate is 0.001mol/L, the concentration of carboxymethyl curdlan gum is 0.001g/mL, controlling its pH scope is 6～8, the dark place lucifuge mixes under the room temperature, solution being placed wavelength is illumination 24h under the 365nm uviol lamp again, obtain faint yellow nano silver colloid aqueous solution, transmission electron microscope results as shown in Figure 6, the particle diameter of nano-Ag particles on average is about 20nm.
Embodiment 7
The 0.43g silver nitrate is dissolved in deionized water, and constant volume is in the brown volumetric flask of 50mL, and preparation concentration is the 0.05mol/L silver nitrate aqueous solution; With 0.02g carboxymethyl curdlan gum (M
w≈ 800,000) be dissolved in the 20mL deionized water, preparation concentration is the carboxymethyl curdlan gum aqueous solution of 0.1g/mL; With 0.2mL silver nitrate aqueous solution and 2.5mL carboxymethyl curdlan gum aqueous solution, adding deionized water, to make overall solution volume be 5mL again, wherein the concentration of silver nitrate is 0.002mol/L, the concentration of carboxymethyl curdlan gum is 0.05g/mL, controlling its pH scope is 6～8, and the dark place lucifuge mixes under the room temperature, and solution being placed wavelength is illumination 24h under the 365nm uviol lamp again, obtain the rufous nano silver colloid aqueous solution, the particle diameter of prepared nano-Ag particles on average is about 100nm.
Embodiment 8
The 0.43g silver nitrate is dissolved in deionized water, and constant volume is in the brown volumetric flask of 50mL, and preparation concentration is the 0.05mol/L silver nitrate aqueous solution; With 0.02g carboxymethyl curdlan gum (M
w≈ 800,000) be dissolved in the 20mL deionized water, preparation concentration is the carboxymethyl curdlan gum aqueous solution of 0.1g/mL; With 0.4mL silver nitrate aqueous solution and 0.5mL carboxymethyl curdlan gum aqueous solution, adding deionized water, to make overall solution volume be 5mL again, wherein the concentration of silver nitrate is 0.004mol/L, the concentration of carboxymethyl curdlan gum is 0.01g/mL, controlling its pH scope is 6～8, and the dark place lucifuge mixes under the room temperature, and solution being placed wavelength is illumination 24h under the 365nm uviol lamp again, obtain the yellowish-brown nano silver colloid aqueous solution, the particle diameter of prepared nano-Ag particles on average is about 60nm.
Embodiment 9
The 0.85g silver nitrate is dissolved in deionized water, and constant volume is in the brown volumetric flask of 50mL, and preparation concentration is the 0.1mol/L silver nitrate aqueous solution; With 0.1g carboxymethyl curdlan gum (M
w≈ 800,000) be dissolved in the 10mL deionized water, preparation concentration is the carboxymethyl curdlan gum aqueous solution of 1g/mL; With 0.5mL silver nitrate aqueous solution and 1mL carboxymethyl curdlan gum aqueous solution, adding deionized water, to make overall solution volume be 5mL again, wherein the concentration of silver nitrate is 0.01mol/L, the concentration of carboxymethyl curdlan gum is 0.1g/mL, controlling its pH scope is 6～8, the dark place lucifuge mixes under the room temperature, solution being placed wavelength is illumination 24h under the 365nm uviol lamp again, obtain brown nano silver colloid aqueous solution, transmission electron microscope results as shown in Figure 7, the particle diameter of prepared nano-Ag particles on average is about 150nm.
Claims (1)
1. colloid aqueous solution preparation method who contains nano-Ag particles based on the carboxymethyl curdlan gum polysaccharide, it is characterized in that, by with silver nitrate aqueous solution and carboxymethyl curdlan gum aqueous solution and wherein the concentration of silver nitrate be 0.001-0.01 mol/L, the concentration of carboxymethyl curdlan gum is 0.001-0.1g/mL, through obtaining containing the nano silver colloid aqueous solution of different-grain diameter and particle diameter distribution behind the ultraviolet irradiation;
Described mixing refers to: control pH scope was 6 ~ 8 and adopts under the lucifuge environment and stir after described two kinds of solution were mixed;
Described ultraviolet irradiation refers to: illumination 1-24h under the uviol lamp of employing wavelength X=365nm;
The molecular weight of described carboxymethyl curdlan gum is 90,000-800,000;
The average grain diameter of described nano silver colloid aqueous solution is 10-100nm.
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| US9403995B2 (en) | 2010-11-02 | 2016-08-02 | Indian Institute Of Technology | Blue coloured aqueous dispersion of silver nanoparticles a process for preparation and compositions thereof |
| CN102921958B (en) * | 2012-11-06 | 2014-10-15 | 上海交通大学 | Method for preparing luminous nano-silver with pH adjusting phase transfer behaviors |
| CN103305063B (en) * | 2013-05-29 | 2015-09-30 | 武汉理工大学 | A kind of preparation method of curdlan-nano-copper compound antibacterial gel |
| CN103480859B (en) * | 2013-09-24 | 2016-01-27 | 江苏大学 | A kind of preparation method of polysaccharide-based Nano silver grain |
| CN103752847B (en) * | 2014-01-25 | 2016-03-02 | 华南理工大学 | A kind of fast preparation method of hemicellulose/nano silver colloidal sol |
| CN104174868B (en) * | 2014-08-24 | 2016-06-22 | 湖南科技大学 | A kind of method preparing water-soluble silver nano-cluster with ultraviolet light reduction silver ammino solution |
| CN104368823A (en) * | 2014-10-22 | 2015-02-25 | 苏州正业昌智能科技有限公司 | Method for preparing nano-silver colloidal solution |
| CN106188574B (en) * | 2016-07-18 | 2018-11-20 | 上海交通大学 | A kind of carboxymethyl curdlan aqueous solution or hydrogel and its preparation method and application |
| CN106519060A (en) * | 2016-09-22 | 2017-03-22 | 江南大学 | Preparation of carboxymethyl curdlan |
| KR102033545B1 (en) * | 2017-06-05 | 2019-10-17 | 대주전자재료 주식회사 | Silver particle and method of manufacture thereof |
| CN108213459B (en) * | 2018-03-14 | 2020-12-29 | 郑州轻工业学院 | Preparation method of glucan/nano gold-silver alloy compound |
| KR102308468B1 (en) * | 2018-12-28 | 2021-10-06 | 대주전자재료 주식회사 | Spherical silver powder and preparation method thereof |
| CN110181037B (en) * | 2019-05-17 | 2021-04-06 | 云南玖香鲜花生物科技股份有限公司 | Silver nano-particles and preparation method thereof |
| CN115415538A (en) * | 2022-07-21 | 2022-12-02 | 苏州北美国际高级中学 | Antibacterial nano silver and rapid preparation method thereof |
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