CN101450385A - Nano silver colloid aqueous solution preparation method using sodium cellulose glycolate - Google Patents
Nano silver colloid aqueous solution preparation method using sodium cellulose glycolate Download PDFInfo
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- CN101450385A CN101450385A CNA2008101546987A CN200810154698A CN101450385A CN 101450385 A CN101450385 A CN 101450385A CN A2008101546987 A CNA2008101546987 A CN A2008101546987A CN 200810154698 A CN200810154698 A CN 200810154698A CN 101450385 A CN101450385 A CN 101450385A
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Abstract
The invention discloses a method for preparing a nanometer silver colloid aqueous solution by adopting sodium carboxymethyl cellulose. The method comprises the following steps: a silver nitrate solid is dissolved in deionized water so as to prepare a silver nitrate aqueous solution A; sodium carboxymethyl cellulose is dissolved in deionized water so as to prepare a solution B; the solution A and the solution B are mixed, wherein the concentration of silver nitrate is 5*10<-5>-2.5*10<-2> mol/l, and the concentration of the sodium carboxymethyl cellulose is 0.2 to 25 g/l; the pH value of the solutions is controlled between 7 and 11; and the solutions react for 2 to 20 hours at a temperature between 15 and 90 DEG C, so as to obtain the aqueous solution containing silver colloid particles with the average particle size less than 100 nanometers. The nanometer silver colloid aqueous solution obtained by the method is brownish-grey at high concentration and is transparent bright yellow after dilution. The prepared nanometer silver colloid particles are stable in shape, good in dispersibility, adjustable and controllable in particle size distribution. The method has the advantages that the method adopts a common reaction vessel for reaction, and is simple in process, little in equipment investment and easy to implement, and raw materials involved in the reaction are friendly to environment, free from pollution, few in product impurities and convenient for post-treatment.
Description
Technical field
The invention discloses a kind of method that adopts sodium carboxymethylcellulose to prepare nano silver colloid aqueous solution; under temperate condition; prepare simultaneously the green chemistry process of nano silver colloid aqueous solution with sodium carboxymethylcellulose, belong to medical sterilization, metal photoelectricity and catalytic nanometer functional material synthesis technical field as chemical reducing agent and protective agent.
Background technology
In recent years, along with the extensive use of Nano Silver material in fields such as superconduction, antibiotic, biological, catalysis, microelectronics and photonic crystals, its relevant various technologies of preparing have also obtained developing rapidly.Liquid phase chemical reduction law theory system of the present invention is complete, and Equipment Foundations are good, the process conditions maturation, easily controls, and has remarkable advantages such as speed of production is fast, output is big, productive rate is high, cost is low, is well suited for industrialized production.
Be equipped with in the practical systems of nano silver colloid particle a typical liquid phase chemical reduction legal system that adopts, include basic comprising unit such as solvent, argentiferous presoma, reducing agent and protective agent at least; Solvent wherein can be certain organic matter, also can be common deionized water or distilled water; The argentiferous presoma is generally certain silver salt, as silver nitrate, silver perchlorate; Reducing agent both can be that organic matter also can be an inorganic matter; as organic certain alcohol, phenol, aldehyde or inorganic hydrazine hydrate, sodium borohydride; protective agent then is generally the organic macromolecule of long-chain, as dodecyl sodium sulfate, CTAB, PVP etc.From disclosed various documents and patent at present; though it is quite a lot to cooperate various reducing agents and protective agent to prepare the method for nano silver colloid and powder, mostly do not resolve distribute contradiction between many requirements such as control, appliance arrangement input, succinct system formation, green chemistry process of particle diameter.As disclosing a kind of method that adopts sodium carboxymethylcellulose to prepare simultaneously nano-Ag particles among the Chinese patent CN101121203A as reducing agent and protective agent, but the molecular weight ranges of its employed sodium carboxymethylcellulose is not quite clear, prepare also heterogeneity of the particle size of product and form, in implementation process, also need to use extra microwave heating equipment, be unfavorable for industrialized production; Though the described method of Chinese patent CN1686646A can obtain the controlled single dispersed nano silver particle of particle diameter by aqueous systems, preparation process needs to carry out under Vltrasonic device and high-speed stirred are auxiliary, has increased the input of equipment; A simple and " green " the method for the synthesis of Au of 2006 the 8th phases of GreenChemistry periodical that Britain imperial family chemistry can be published; Ag; disclosing a kind of employing glucose in andAu-Ag alloy nanoparticles one literary composition is that reducing agent, soluble starch are protectant Preen nono silver granule preparing process; but, thereby on considering, the terseness of cost control and method has shortcoming because reducing agent and protective agent have used two kinds of different materials respectively.Disclosed Nano Silver preparation method then relates to a large amount of uses of organic solutions such as environmentally harmful reducing agent hydrazine hydrate and thiacyclohexane in Chinese patent CN101121204A and CN1759962A.
What the method for addressing with above document was different is, the technical scheme that proposes among the present invention not only can be in common reaction vessel gentle enforcement, and under certain process conditions, can prepare the mono-dispersed nano silver colloidal particles; Employed sodium carboxymethylcellulose is a kind of generally acknowledged eco-friendly chemical substance, and it can also play the protective agent effect, thereby reduce raw-material input when using as reducing agent, has reduced cost.Because raw material itself green is harmless, the solvent deionized water environmentally safe, thereby meet the requirement of sustainable development.
Summary of the invention
The object of the present invention is to provide a kind of under temperate condition the green technological process of the controlled nano silver colloid aqueous solution of preparation size.The nano silver colloid aqueous solution that adopts this method to obtain is taupe during high concentration, and the dilution back is transparent glassy yellow; Prepared nano silver colloid particle shape is stable, favorable dispersibility, and particle diameter distributes adjustable, controlled; The common response container is adopted in reaction, and process is simple, the equipment less investment, easily implement, related raw material environmental friendliness, pollution-free in the reaction, and impurity in products is few, is easy to post processing.
The present invention is realized by following technical proposals:
The present invention adopts sodium carboxymethylcellulose to prepare nano silver colloid aqueous solution, and concrete grammar is: the silver nitrate solid is dissolved in the deionized water, and preparation obtains silver nitrate aqueous solution A, and its molar concentration is 0.01-5mol/L; Sodium carboxymethylcellulose is dissolved preparation obtain solution B in deionized water, its concentration is 0.2-25g/L; A, B two solution are mixed, and wherein the concentration of silver nitrate is 5 * 10
-5-2.5 * 10
-2Mol/L, sodium carboxymethylcellulose concentration is 0.2-25g/L, controls its pH value between 7-11, obtains containing the aqueous solution of average grain diameter less than the silver colloidal particles of 100 nanometers in reaction under 15-90 ℃ after 2-20 hour.
Described sodium carboxymethylcellulose double as reducing agent and protective agent, molecular weight ranges is chosen in 90, and 000-250 is between 000.
Advantage of the present invention is:
Adopt the nano silver colloid particle shape of the present invention's preparation stable, favorable dispersibility, the sodium carboxymethylcellulose that adds different molecular weight can produce significantly influence, the particle diameter distribution easy-regulating of product to the size of silver nano-grain; When the molecular weight of selected sodium carboxymethylcellulose is,, can prepare mono-dispersed nano silver particle at 90,000 o'clock by regulating technological parameter; Polysaccharide macro-molecular reducing agent sodium carboxymethylcellulose double as protective agent uses, and has both saved unnecessary extra raw material input, has purified final products again, and single step reaction can obtain required the nano silver colloid particle and the aqueous solution thereof.Because compound used therefor green, nontoxic, product need not further separation and purification treatment, thereby can directly apply to strict technical fields such as biology, medical science, pharmacy, sterilization; Simultaneously, preparation technology itself is simple, mild condition, easily control, reduction reaction is carried out in the aqueous solution, course of reaction need not Vltrasonic device again, the outer means of heating using microwave single-candidate are auxiliary, reactions steps is few, easy and simple to handle, the input cost of raw material and equipment is low, is convenient to realize large-scale industrial production.
Description of drawings
Fig. 1. the nano-Ag particles transmission electron microscope photo of embodiment 1;
Fig. 2. the nano-Ag particles transmission electron microscope photo of embodiment 2;
Fig. 3. the nano-Ag particles transmission electron microscope photo of embodiment 3;
Fig. 4. the single dispersed nano silver particle transmission electron microscope photo of embodiment 4;
Fig. 5. the nano-Ag particles transmission electron microscope photo of embodiment 5.
The specific embodiment
Below in conjunction with embodiment, technology of the present invention and characteristics are described further.
Embodiment 1
The 0.34g silver nitrate joined in the 10mL deionized water make solution A; Reducing agent, the protective agent sodium carboxymethylcellulose (Mw ≈ 90,000) of 0.012g are joined in the 20mL deionized water and dissolve, regulate the pH value between 9-11, make solution B; Get A solution 0.1mL and join in the B solution, under 15 ℃ of conditions the reaction 20 hours, obtain the faint yellow silver colloid aqueous solution, transmission electron microscope results as shown in Figure 1, the silver nano-grain average grain diameter that obtains is less than 60nm.
Embodiment 2
The 0.34g silver nitrate joined in the 10mL deionized water make solution A; Reducing agent, the protective agent sodium carboxymethylcellulose (Mw ≈ 90,000) of 0.012g are joined in the 20mL deionized water, fully stir 30min (rotating speed 200r/min) dissolving after, regulate the pH value between 7-9, make solution B; Get A solution 0.1mL and join in the B solution, place water-bath to be heated to 60 ℃; Continue stirring reaction after 4 hours, obtain the Yellow nanometer silver colloid aqueous solution, transmission electron microscope results as shown in Figure 2, the nano-Ag particles average grain diameter that obtains is less than 100 nanometers.
Embodiment 3
Silver nitrate 0.34g joined be prepared into A liquid in the 10mL deionized water; 0.004g reducing agent, protective agent sodium carboxymethylcellulose (Mw ≈ 90,000) are joined in the 20mL deionized water, fully stir 30min (rotating speed 100r/min) dissolving after, regulate the pH value between 7-9, make solution B; Get A solution 0.1mL and join in the B solution, place water-bath to be heated to 80 ℃; Continue stirring reaction after 4 hours, obtain the Yellow nanometer silver sol aqueous solution, transmission electron microscope results as shown in Figure 3, the nano-Ag particles average grain diameter that obtains is about 30 nanometers.
Embodiment 4
Silver nitrate 0.34g joined be prepared into A liquid in the 10mL deionized water; 0.012g reducing agent, protective agent sodium carboxymethylcellulose (Mw ≈ 90,000) are joined in the 20mL deionized water, fully stir 30min (rotating speed 300r/min) dissolving after, regulate the pH value between 7-9, make solution B; Get A solution 0.1mL and join in the B solution, place water-bath to be heated to 80 ℃; Continue stirring reaction after 4 hours, obtain the Yellow nanometer silver sol aqueous solution, transmission electron microscope results obtains single dispersed nano silver particle average grain diameter and is about 9nm as shown in Figure 4.
Embodiment 5
Silver nitrate 0.34g joined be prepared into A liquid in the 10mL deionized water; 0.02g reducing agent, protective agent sodium carboxymethylcellulose (Mw ≈ 250,000) are joined in the 20mL deionized water, fully stir 30min (rotating speed 300r/min) dissolving after, regulate the pH value between 7-9, make solution B; Get A solution 0.1mL and join in the B solution, place water-bath to be heated to 80 ℃; Continue stirring reaction after 4 hours, obtain the Yellow nanometer silver sol aqueous solution, transmission electron microscope results as shown in Figure 5, the nano-Ag particles average grain diameter that obtains is less than 100nm.
Embodiment 6
Silver nitrate 0.017g joined be prepared into A liquid in the 10mL deionized water; 0.5g reducing agent, protective agent sodium carboxymethylcellulose (Mw ≈ 120,000) are joined in the 20mL deionized water, fully stir 30min (rotating speed 400r/min) dissolving after, regulate the pH value between 7-9, make solution B; Get A solution 0.1mL and join in the B solution, place water-bath to be heated to 80 ℃; Continue stirring reaction after 2 hours, obtain the light yellow nano silver colloidal sol aqueous solution.
Embodiment 7
Silver nitrate 8.5g joined be prepared into A liquid in the 10mL deionized water; 0.25g reducing agent, protective agent sodium carboxymethylcellulose (Mw ≈ 180,000) are joined in the 20mL deionized water, fully stir 30min (rotating speed 200r/min) dissolving after, regulate the pH value between 7-9, make solution B; Get A solution 0.1mL and join in the B solution, place water-bath to be heated to 90 ℃; Continue stirring reaction after 2 hours, obtain the peony nano silver colloidal sol aqueous solution.
The employing sodium carboxymethylcellulose that the present invention proposes prepares the method for nano silver colloid aqueous solution, be described by preferred embodiment, person skilled obviously can be changed or suitably change and combination preparation method as herein described in not breaking away from content of the present invention, spirit and scope, realizes the technology of the present invention.Special needs to be pointed out is, the replacement that all are similar and change apparent to those skilled in the artly, they all are regarded as being included in spirit of the present invention, scope and the content.
Claims (3)
1. method that adopts sodium carboxymethylcellulose to prepare nano silver colloid aqueous solution is characterized in that: the silver nitrate solid is dissolved in the deionized water, and preparation obtains silver nitrate aqueous solution A, and its molar concentration is 0.01-5mol/L; Sodium carboxymethylcellulose is dissolved preparation obtain solution B in deionized water, its concentration is 0.2-25g/L; A, B two solution are mixed, and wherein the concentration of silver nitrate is 5 * 10
-5-2.5 * 10
-2Mol/L, sodium carboxymethylcellulose concentration is 0.2-25g/L, controls its pH value between 7-11, obtains containing the aqueous solution of average grain diameter less than the silver colloidal particles of 100 nanometers in reaction under 15-90 ℃ after 2-20 hour.
2. employing sodium carboxymethylcellulose according to claim 1 prepares the method for nano silver colloid aqueous solution, it is characterized in that described sodium carboxymethylcellulose double as reducing agent and protective agent, and molecular weight ranges is chosen in 90, and 000-250 is between 000.
3. employing sodium carboxymethylcellulose according to claim 1 prepares the method for nano silver colloid aqueous solution; it is characterized in that: with 0.2mol/L silver nitrate 0.1mL; as reducing agent and protectant molecular weight is 90; 000 sodium carboxymethylcellulose 0.012g joins in the 20mL deionized water; after stirring the 30min dissolving; regulate the pH value between 7-9, place water-bath to be heated to 80 ℃ of reactions 4 hours, prepare the single dispersed nano silver particle.
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