CN106041115B - A kind of sodium alginate/silver nanowires colloidal sol and preparation method thereof - Google Patents
A kind of sodium alginate/silver nanowires colloidal sol and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of sodium alginate/silver nanowires colloidal sols and preparation method thereof, in water phase, using ascorbic acid as reducing agent, and using sodium alginate as soft template, ascorbic acid and AgNO3Redox reaction occurs, obtains sodium alginate/silver nanowires colloidal sol.The present invention uses the food-grade sodium alginate of low toxicity as green soft template, using ascorbic acid as reducing agent, silver nanowires colloidal sol is quickly prepared (at 25 DEG C~90 DEG C of low temperature environment) in water phase, the use of organic solvent, dispersing agent, other toxic chemical reducing agents and stabilizer is avoided, it is environmentally protective.Obtained sodium alginate/silver nanowires colloidal sol has important research and application value in fields such as biology, medical treatment, electronics.The silver nanowires outer layer covers that the present invention prepares sodium alginate, can be dispersed in ethyl alcohol or water, solve the problems, such as that silver nanowires easily reunites, is difficult to disperse.
Description
Technical field
The invention belongs to field of nanometer technology, and in particular to a kind of green preparation side of sodium alginate/silver nanowires colloidal sol
Method.
Background technique
In the research boom of nano material, noble metal with its unique light, electricity, catalysis, etc. characteristic and by
Extensive concern.With the development of nanotechnology, synthesis and the characterization method of nano material are constantly improve, the noble metal of different morphologies
Nanostructure is synthesized in succession.Wherein one-dimensional metal nanostructure is due to the properties such as its excellent electricity, optics, magnetics and calorifics
Nano electron device and in terms of have very big application prospect.Silver nanowires, especially diameter are uniform, it is higher to have
The nano wire of draw ratio, catalysis, electronics, optical device, sensor and in terms of have and potential answer
Use prospect.
The preparation method of silver nanowires is varied, is broadly divided into top-down physical method to chemistry from bottom to top
Method, and wherein most commonly used is liquid chemical method.Liquid chemical method can be divided into hard template and soft template method again.Hard template
It needs preparation to meet the template of requirement of experiment before method preparation, needs to post-process template after the reaction was completed.Therefore preparation process is multiple
It is miscellaneous.Soft template method is to prepare silver nanowires under the induction of crystal seed, under the action of the cladding and template effect of surfactant.
Although this method is easy, due to the insufficient residual for being often possible to lead to surfactant of product cleaning, to make to produce
Object band is toxic.At present about the research of the surfactants toxicity such as SDS, PVP.Moreover, the preparation of silver nanowires at present
Either polyol process or microwave method carry out (> 150 DEG C) at relatively high temperatures, largely prepare and answer to limit it
With.
Sodium alginate is a kind of polysaccharide linear polymer extracted from kelp or sargassum, and structure is poly- by Isosorbide-5-Nitrae-
What beta-D-mannuronic acid and α-L- guluronic acid formed, a large amount of carbonyls and hydroxyl are contained in structure, easily formation hydrogen bond.Sea
Mosanom dissolves in water forms viscous liquid, and dissolved-COONa group is dissociated into-COO-And Na+, with multiple negative
The polyion form of charge is present in water, and the microenvironment constituted has suspension well, emulsification and stabilization.Currently,
Sodium alginate is but had not been reported to prepare silver nanowires.
Summary of the invention
The present invention provides a kind of sodium alginate/silver nanowires colloidal sol environment-friendly preparation method thereofs.In water phase, with Vitamin C
Under low temperature (25-90 DEG C) heating condition redox reaction occurs for acid using sodium alginate as soft template as reducing agent,
Stable sodium alginate/silver nanowires colloidal sol can be prepared.
The present invention is realized especially by following technical scheme:
A kind of preparation method of sodium alginate/silver nanowires colloidal sol, in water phase, using ascorbic acid as reducing agent, with
Sodium alginate is as soft template, ascorbic acid and AgNO3Redox reaction occurs, it is molten to obtain sodium alginate/silver nanowires
Glue.
In above-mentioned preparation process, complexing is mainly undergone in the synthesis of silver nanowires, is restored, and nucleation grows four-stage.Specifically
Steps are as follows:
(1) it disperses sodium alginate in ultrapure water, is stirred continuously, the sodium alginate water of 0.1%~5%mg/ml is made
Solution;
(2) above-mentioned sodium alginate aqueous solution is added in ascorbic acid, stirs to it and is dissolved in above-mentioned system;
(3) AgNO is added in the above system3Afterwards, it is placed under room temperature or oil bath or microwave condition and carries out redox
Reaction.The ascorbic acid and AgNO3Molar ratio be 1:1~1.2:1.
The sodium alginate and AgNO3Molar ratio be 0.1:1~5:1, preferred ratio be 0.5:1~5:1.
The reaction temperature is 30 DEG C~90 DEG C, and the reaction time is 0.5~12h.The preferred reaction time is 3~6h.
When reaction temperature is lower than 50 DEG C, sodium alginate and AgNO3Molar ratio be greater than 1.4:1;When reaction temperature is 50
DEG C~90 DEG C when, sodium alginate and AgNO3Molar ratio be 0.5:1~5:1.
The ascorbic acid and AgNO3Molar ratio be 1:1~1.2:1.
By the obtained multiple centrifuge washing of reaction solution deionized water after step (3) reaction, lower sediment is obtained, as
Sodium alginate/silver nanowires colloidal sol.
The centrifugal condition is that 5-30min is centrifuged at revolving speed 1500rpm-4000rpm, and gained precipitating is dissolved in water or ethyl alcohol
Middle preservation.
The above method preparation sodium alginate/silver nanowires colloidal sol in silver nanowires outer layer covers sodium alginate.
The diameter of the silver nanowires is 50nm-250nm, length is 5-40 μm.
Compared with prior art, the invention has the following advantages that
(1) present invention uses the food-grade sodium alginate of low toxicity as green soft template, using ascorbic acid as reducing agent,
Quick preparation silver nanowires colloidal sol (at 25 DEG C~90 DEG C of low temperature environment) in water phase, avoids that organic solvent, dispersing agent, other have
The use of malicious chemical reducing agent and stabilizer, it is environmentally protective.Obtained sodium alginate/silver nanowires colloidal sol is in biology, medical treatment, electricity
There are important research and application value in the fields such as son.
(2) the silver nanowires outer layer covers prepared of the present invention sodium alginate, can be dispersed in ethyl alcohol or water,
Solve the problems, such as that silver nanowires easily reunites, is difficult to disperse.
(3) present invention prepares silver nanowires colloidal sol using sodium alginate as soft template, can advantageously promote sodium alginate
Functionalization and higher value application, also the research on utilization for agricultural-forestry biomass resource opens new research direction.
(4) present invention prepares silver nanowires using biomaterial, provides new approaches for the preparation of silver nanowires, is big
Amount green production silver nanowires provides possibility.
Detailed description of the invention
Fig. 1 (A) (B) (C) (D) is respectively sodium alginate/silver nanowires colloidal sol SEM figure of 1-4 of the embodiment of the present invention.
Fig. 2 (A) (B) (C) (D) is respectively sodium alginate/silver nanowires colloidal sol SEM figure of 5-8 of the embodiment of the present invention.
Fig. 3 (A) (B) is respectively sodium alginate/silver nanowires colloidal sol SEM figure of the embodiment of the present invention 9 and 10.
Specific embodiment
The present invention is further explained in the light of specific embodiments, but not limited to this.
Embodiment 1
0.174g sodium alginate is weighed in 100ml ultrapure water, is stirred continuously to form uniform sodium alginate soln.?
The ascorbic acid of 0.315g is added in the state of stirring, the AgNO of 0.275g is added after dissolving it all3, so that sodium alginate
With AgNO3Molar ratio be 0.5:1.It is placed reaction liquid into the state of continuously stirring in 30 DEG C of oil baths and reacts 6h, measure UV-
Vis spectrum.
Solution after reaction is centrifuged 20min at revolving speed 2000rpm, absorbs supernatant liquor, retains precipitating, and repeatedly use
Deionized water centrifuge washing, until supernatant is colorless and transparent.Resulting precipitating is placed in deionized water or dehydrated alcohol
It saves.
Embodiment 2
0.35g sodium alginate is weighed in 100ml ultrapure water, is stirred continuously to form uniform sodium alginate soln.?
The ascorbic acid of 0.315g is added in the state of stirring, the AgNO of 0.275g is added after dissolving it all3, so that sodium alginate
With AgNO3Molar ratio be 1:1.It is placed reaction liquid into the state of continuously stirring in 30 DEG C of oil baths and reacts 6h, measure UV-
Vis spectrum.
Solution after reaction is centrifuged 20min at revolving speed 2000rpm, absorbs supernatant liquor, retains precipitating, and repeatedly use
Deionized water centrifuge washing, until supernatant is colorless and transparent.Resulting precipitating is placed in deionized water or dehydrated alcohol
It saves.
Embodiment 3
0.49g sodium alginate is weighed in 100ml ultrapure water, is stirred continuously to form uniform sodium alginate soln.?
The ascorbic acid of 0.315g is added in the state of stirring, the AgNO of 0.275g is added after dissolving it all3, so that sodium alginate
With AgNO3Molar ratio be 1.4:1.It is placed reaction liquid into the state of continuously stirring in 30 DEG C of oil baths and reacts 6h, measure UV-
Vis spectrum.
Solution after reaction is centrifuged 20min at revolving speed 2000rpm, absorbs supernatant liquor, retains precipitating, and repeatedly use
Deionized water centrifuge washing, until supernatant is colorless and transparent.Resulting precipitating is placed in deionized water or dehydrated alcohol
It saves.
Embodiment 4
0.66g sodium alginate is weighed in 100ml ultrapure water, is stirred continuously to form uniform sodium alginate soln.?
The ascorbic acid of 0.315g is added in the state of stirring, the AgNO of 0.275g is added after dissolving it all3, so that sodium alginate
With AgNO3Molar ratio be 1.9:1.It is placed reaction liquid into the state of continuously stirring in 30 DEG C of oil baths and reacts 6h, measure UV-
Vis spectrum.
Solution after reaction is centrifuged 20min at revolving speed 2000rpm, absorbs supernatant liquor, retains precipitating, and repeatedly use
Deionized water centrifuge washing, until supernatant is colorless and transparent.Resulting precipitating is placed in deionized water or dehydrated alcohol
It saves.
Embodiment 5
0.174g sodium alginate is weighed in 100ml ultrapure water, is stirred continuously to form uniform sodium alginate soln.?
The ascorbic acid of 0.315g is added in the state of stirring, the AgNO of 0.275g is added after dissolving it all3, so that sodium alginate
With AgNO3Molar ratio be 0.5:1.It is placed reaction liquid into the state of continuously stirring in 70 DEG C of oil baths and reacts 6h, measure UV-
Vis spectrum.
Solution after reaction is centrifuged 20min at revolving speed 2000rpm, absorbs supernatant liquor, retains precipitating, and repeatedly use
Deionized water centrifuge washing, until supernatant is colorless and transparent.Resulting precipitating is placed in deionized water or dehydrated alcohol
It saves.
Embodiment 6
0.35g sodium alginate is weighed in 100ml ultrapure water, is stirred continuously to form uniform sodium alginate soln.?
The ascorbic acid of 0.315g is added in the state of stirring, the AgNO of 0.275g is added after dissolving it all3, so that sodium alginate
With AgNO3Molar ratio be 1:1.It is placed reaction liquid into the state of continuously stirring in 70 DEG C of oil baths and reacts 6h, measure UV-
Vis spectrum.
Solution after reaction is centrifuged 20min at revolving speed 2000rpm, absorbs supernatant liquor, retains precipitating, and repeatedly use
Deionized water centrifuge washing, until supernatant is colorless and transparent.Resulting precipitating is placed in deionized water or dehydrated alcohol
It saves.
Embodiment 7
0.49g sodium alginate is weighed in 100ml ultrapure water, is stirred continuously to form uniform sodium alginate soln.?
The ascorbic acid of 0.315g is added in the state of stirring, the AgNO of 0.275g is added after dissolving it all3, so that sodium alginate
With AgNO3Molar ratio be 1.4:1.It is placed reaction liquid into the state of continuously stirring in 70 DEG C of oil baths and reacts 6h, measure UV-
Vis spectrum.
Solution after reaction is centrifuged 20min at revolving speed 2000rpm, absorbs supernatant liquor, retains precipitating, and repeatedly use
Deionized water centrifuge washing, until supernatant is colorless and transparent.Resulting precipitating is placed in deionized water or dehydrated alcohol
It saves.
Embodiment 8
0.66g sodium alginate is weighed in 100ml ultrapure water, is stirred continuously to form uniform sodium alginate soln.?
The ascorbic acid of 0.315g is added in the state of stirring, the AgNO of 0.275g is added after dissolving it all3, so that sodium alginate
With AgNO3Molar ratio be 1.9:1.It is placed reaction liquid into the state of continuously stirring in 70 DEG C of oil baths and reacts 6h, measure UV-
Vis spectrum.
Solution after reaction is centrifuged 20min at revolving speed 2000rpm, absorbs supernatant liquor, retains precipitating, and repeatedly use
Deionized water centrifuge washing, until supernatant is colorless and transparent.Resulting precipitating is placed in deionized water or dehydrated alcohol
It saves.
Embodiment 9
0.174g sodium alginate is weighed in 100ml ultrapure water, is stirred continuously to form uniform sodium alginate soln.?
The ascorbic acid of 0.315g is added in the state of stirring, the AgNO of 0.275g is added after dissolving it all3, so that sodium alginate
With AgNO3Molar ratio be 0.5:1.It is placed reaction liquid into the state of continuously stirring in 50 DEG C of oil baths and reacts 3h, measure UV-
Vis spectrum.
Solution after reaction is centrifuged 20min at revolving speed 2000rpm, absorbs supernatant liquor, retains precipitating, and repeatedly use
Deionized water centrifuge washing, until supernatant is colorless and transparent.Resulting precipitating is placed in deionized water or dehydrated alcohol
It saves.
Embodiment 10
0.66g sodium alginate is weighed in 100ml ultrapure water, is stirred continuously to form uniform sodium alginate soln.?
The ascorbic acid of 0.315g is added in the state of stirring, the AgNO of 0.275g is added after dissolving it all3, so that sodium alginate
With AgNO3Molar ratio be 1.9:1.It is placed reaction liquid into the state of continuously stirring in 50 DEG C of oil baths and reacts 3h, measure UV-
Vis spectrum.
Solution after reaction is centrifuged 20min at revolving speed 2000rpm, absorbs supernatant liquor, retains precipitating, and repeatedly use
Deionized water centrifuge washing, until supernatant is colorless and transparent.Resulting precipitating is placed in deionized water or dehydrated alcohol
It saves.
Sodium alginate/silver nanowires colloidal sol SEM that Fig. 1 is 1-4 of the embodiment of the present invention schemes.As seen from the figure, in 30 DEG C of feelings
Under condition, there is silver nanowires in Examples 1 and 2, the Yin Na with the increase of sodium alginate amount, in embodiment 3 and 4
The content of rice noodles gradually increases, and illustrates that sodium alginate plays important function to the generation of final silver nanowires.
Sodium alginate/silver nanowires colloidal sol SEM that Fig. 2 is 5-8 of the embodiment of the present invention schemes.As seen from the figure, at 70 DEG C
In the case of, there are many silver nanowiress in embodiment 5-8, diameter is about 50nm-250nm, length is between 5-40 μm.
Fig. 3 is that sodium alginate/silver nanowires colloidal sol SEM of the embodiment of the present invention 9 and 10 schemes.As seen from the figure, at 50 DEG C
In the case of, many silver nanowiress are generated in embodiment 9 and 10.Its diameter is about 50nm-250nm, length is between 5-40 μm.
A large amount of silver nano-grains are existed simultaneously in above-described embodiment solution, it is therefore desirable to which centrifuge separation is purer to obtain
Silver nanowires colloidal sol.
Claims (10)
1. a kind of sodium alginate/silver nanowires colloidal sol preparation method, which is characterized in that specific step is as follows:
(1) it disperses sodium alginate in ultrapure water, is stirred continuously, the sodium alginate aqueous solution of 0.1%~5%mg/ml is made;
(2) above-mentioned sodium alginate aqueous solution is added in ascorbic acid, stirs to it and is dissolved in above-mentioned system;
(3) AgNO is added in the above system3Afterwards, redox reaction is carried out under the conditions of being placed in 30 DEG C~70 DEG C, the reaction time is
0.5~12h, the sodium alginate and AgNO3Molar ratio be 0.1:1~5:1.
2. preparation method according to claim 1, which is characterized in that the sodium alginate and AgNO3Molar ratio be 0.5:
1~5:1.
3. preparation method according to claim 2, which is characterized in that when reaction temperature be lower than 50 DEG C when, sodium alginate with
AgNO3Molar ratio be greater than 1.4:1;When reaction temperature is 50 DEG C~70 DEG C, sodium alginate and AgNO3Molar ratio be 0.5:1
~5:1.
4. preparation method according to claim 1 or 2 or 3, which is characterized in that the ascorbic acid and AgNO3Molar ratio
For 1:1~1.2:1.
5. preparation method according to claim 1 or 2 or 3, which is characterized in that the reaction time is 3~6h.
6. preparation method according to claim 1 or 2 or 3, which is characterized in that will be obtained anti-after step (3) reaction
The multiple centrifuge washing of liquid deionized water is answered, lower sediment, as sodium alginate/silver nanowires colloidal sol are obtained.
7. preparation method according to claim 6, which is characterized in that the centrifugal condition is in revolving speed 1500rpm-
5-30min is centrifuged under 4000rpm, gained precipitating, which is dissolved in water or ethyl alcohol, to be saved.
8. preparation method according to claim 5, which is characterized in that use obtained reaction solution after step (3) reaction
The multiple centrifuge washing of deionized water obtains lower sediment, as sodium alginate/silver nanowires colloidal sol.
9. sodium alginate made from claim 1~8 any one the method/silver nanowires colloidal sol, which is characterized in that described
In sodium alginate/silver nanowires colloidal sol silver nanowires outer layer covers sodium alginate.
10. sodium alginate according to claim 9/silver nanowires colloidal sol, which is characterized in that the diameter of the silver nanowires
It is 5-40 μm for 50nm-250nm, length.
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CN106601339A (en) * | 2016-12-20 | 2017-04-26 | 上海交通大学 | Method for preparing silver nanowire and alginate composite transparent conductive film |
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