CN106735292A - A kind of preparation method of starch/silver nanoparticle compound particle - Google Patents
A kind of preparation method of starch/silver nanoparticle compound particle Download PDFInfo
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- CN106735292A CN106735292A CN201611101560.1A CN201611101560A CN106735292A CN 106735292 A CN106735292 A CN 106735292A CN 201611101560 A CN201611101560 A CN 201611101560A CN 106735292 A CN106735292 A CN 106735292A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
Abstract
The present invention provides a kind of preparation method of starch/silver compound particle, the described method comprises the following steps：(1) silver-colored precursor water solution is provided；(2) starch granules aqueous dispersions are provided；(3) reducing agent aqueous solution is provided；(4) the starch granules aqueous dispersions are well mixed with the silver-colored precursor water solution, and vibrate or stir at least 30 minutes；(5) reducing agent aqueous solution is added to the mixture of gained in step (4), the pH of regulation system to 3~13, and reacted at a temperature of 25~60 DEG C, then obtain starch/silver nanoparticle compound particle solid powder through being centrifuged, washing and dry.The inventive method is that this can further simplify the preparation process of supported silver nano-particle, it is easy to industrialize without carrying out any surface modification, modified and functionalization to starch granules.
Description
Technical field
The invention belongs to feature hybrid field of nanometer material technology, in particular it relates to a kind of starch/silver is compound
The preparation method of particle.
Technical background
Due to its minimum size and larger specific surface area, Nano silver grain has completely not compared with bulk metal silver
Same physics and chemical property, have therefore suffered from the concern of more and more scientific workers.In recent years, Nano silver grain by
It is widely used in the fields such as biology sensor, catalysis, antibacterial and Surface-enhanced spectroscopic.But, due to larger surface
Can, Nano silver grain is susceptible to irreversible aggregation and reduces or even lose related activity.In order to solve the above problems, by silver
Nano-particle is fixed on carrier, is prepared the nano composite material containing Nano silver grain and is had become a kind of effective hand
Section.
Up to the present, inorganic matter and synthesis macromolecule are mainly included for loading the carrier of Nano silver grain.In recent years,
The natural polymer subcarrier of low cost, good biocompatibility and wide material sources causes extensive concern.Wherein, researcher
Notice is concentrated mainly on cellulose carrier, although realize the successful load of Nano silver grain, but in most of reactions
It is middle to be aided with more harsh reaction condition or surface preparation must be carried out to cellulose carrier, so as to effectively improve its
Dispersity in medium is improving the load of Nano silver grain.
For example, H.Liu etc. is natural polymer subcarrier with carboxy-modified Cellulose nanocrystal, band is made using electrostatic interaction
The silver ion of positive electricity is adsorbed onto the surface of aforementioned bearer, then causes that Nano silver grain loads to fibre by the way of in-situ reducing
The nanocrystalline surface of dimension element is (referring to " Preparation of silver nanoparticles on cellulose
nanocrystals and the application in electrochemical detection of DNA
hybridization”,Cellulose,2011,18,67–74).In the method for H.Liu et al., the table of Cellulose nanocrystal
Face carboxylated plays vital effect to the Nano silver grain for successfully preparing Cellulose nanocrystal load.
Again for example, Rezayat etc. is in subcritical-supercritical CO2Atmosphere in synthesized the noble metal nano particles such as silver, palladium
The Cellulose nanocrystal compound particle of load is (referring to " Green one-step synthesis of catalytically
active palladium nanoparticles supported on cellulose nanocrystals”,Acs
Sustainable Chemistry&Engineering,2014,2,1241-1250).Specifically, by silver and palladium noble metal precursor
Body mixes with Cellulose nanocrystal, is placed in high-pressure sterilizing pot, is passed through CO2, silver and palladium are synthesized in the environment of high pressure and high temperature
The Cellulose nanocrystal compound particle of nanometer particle load, wherein, the reaction condition of HTHP is that silver and Pd nano particle exist
The important guarantee loaded in Cellulose nanocrystal.
Therefore, because the existing synthetic method in natural polymer supported on carriers Nano silver grain is relatively complicated, instead
Answer condition more harsh, need exist for providing the method in natural polymer supported on carriers Nano silver grain.
The content of the invention
Therefore, it is an object of the invention to propose a kind of simple to operate, low production cost and can industrialized production shallow lake
The preparation method of powder/silver nanoparticle compound particle.
The purpose of the present invention is achieved through the following technical solutions.
The invention provides a kind of preparation method of starch/silver compound particle, the described method comprises the following steps：
(1) silver-colored precursor water solution is provided；
(2) starch granules aqueous dispersions are provided；
(3) reducing agent aqueous solution is provided；
(4) the starch granules aqueous dispersions are well mixed with the silver-colored precursor water solution, and vibrate or stir extremely
It is few 30 minutes；
(5) reducing agent aqueous solution is added to the mixture of gained in step (4), the pH of regulation system to 3~13,
And reacted at a temperature of 25~60 DEG C, then obtain starch/silver nanoparticle compound particle solid powder through being centrifuged, washing and dry
End.
It is not intended to bound by theory, it is believed that, the surface of starch granules carries negative electrical charge in the present invention, and silver-colored in step (1)
Silver-colored ammonium ion carries positive charge in precursor solution such as silver ammino solution.In mixed process, based on electrostatic interaction, silver-colored ammonia from
Son will be adsorbed onto the surface of starch granules.Then, adding PVP carries out in-situ reducing, obtains starch/silver
Nano-complex particle.
In the preparation process of starch/silver nanoparticle compound particle, without starch granules is carried out any surface it is modified with
Functionalization, preparation process was not only simple but also controllable, and starch granules source is wide and low cost, is suitable for industrialized production.
According to the method that the present invention is provided, wherein, the silver-colored precursor solution is selected from silver nitrate aqueous solution, triethanolamine silver
Solution, the silver acetate aqueous solution and silver ammino solution etc..In preferred embodiments, the silver-colored precursor solution is that silver-colored ammonia is molten
Liquid.
According to the method that the present invention is provided, wherein, the concentration of silver ion is generally not more than 0.5 in the silver-colored precursor solution
Mol/L.In some embodiments, the concentration of silver ion is 0.001~0.2 mol/L in silver-colored precursor solution, at some
It is 0.001~0.02 mol/L in embodiment, and is in some embodiments 0.01~0.02 mol/L.
In preferred embodiments, silver-colored precursor solution is silver ammino solution in step (1), and its concentration is not higher than 0.5
Mol/L.In some specific embodiments, silver ammino solution concentration range is 0.001~0.2 mol/L, in some embodiment party
It is 0.001~0.02 mol/L in case, and is 0.01~0.02 mol/L in some specific embodiments.
In the present invention, the starch granules wide material sources can be carried by alkali carries, acid and the mode such as put forward with enzyme and obtain.
In preferred embodiments, the starch granules can be with potato, wheat, tomato, sweet potato and seed
The root and/or stem of the green plantss such as amaranth are raw material by obtained in alkaline extraction.In some specific embodiments, the starch
Grain takes from Grain Production of Amaranthus seed.In addition, the starch granules used in the present invention directly can also be bought by market obtaining.
According to the preparation method that the present invention is provided, wherein, the starch granules is modified without any, particularly without chemistry
It is modified.
According to the preparation method that the present invention is provided, wherein, the consumption of the starch granules is silver weight in silver-colored precursor solution
1~200 times of amount.In some embodiments, the consumption of the starch granules is 1~50 of silver-colored weight in silver-colored precursor solution
Times；It is in some embodiments 1.5~10 times of silver-colored weight in silver-colored precursor solution；And in some specific embodiments
It is 1.75~9.5 times of silver-colored weight in silver-colored precursor solution.
According to the preparation method that the present invention is provided, wherein, the concentration of starch granules aqueous dispersions is not generally high in step (2)
In 0.1 grams per milliliter.In some embodiments, in step (2) starch granules aqueous dispersions concentration for 0.002~0.02 gram/
Milliliter, is in some embodiments 0.005~0.015 grams per milliliter, and is in some embodiments 0.01 grams per milliliter.
According to the preparation method that the present invention is provided, wherein, the average-size of starch granules is 100 nanometers~2000 nanometers.
In some embodiments, the average-size of starch granules is 500 nanometers~1000 nanometers, and in some embodiments,
The average-size of starch granules is for about 900 nanometers.
According to the preparation method that the present invention is provided, wherein, the reducing agent is selected from trisodium citrate, sodium borohydride, boron hydrogen
Change potassium, hydroxylamine hydrochloride, formaldehyde, hydrazine, tannic acid, sodium hypophosphite, PVP, methyl alcohol, ethanol, propyl alcohol, ascorbic acid
With one or more in THPC.In some specific embodiments, the reducing agent is polyvinylpyrrolidine
Alkanone.
According to the preparation method that the present invention is provided, wherein, the consumption of the reducing agent can be the 0.6 of silver-colored forerunner's body weight
~600 times.In some embodiments, the consumption of the reducing agent can be 0.6~60 times of silver-colored forerunner's body weight；In some realities
Apply in scheme as 5~10 times；And in some specific embodiments be 6 times.
In some embodiments, reductant solution is the ethanol solution of PVP in step (3), and its
Concentration is not higher than 0.5 grams per milliliter.In some specific embodiments, the concentration model of the ethanol solution of PVP
It is 0.002~0.1 grams per milliliter to enclose, and is 0.01~0.1 grams per milliliter in some specific embodiments, in some specific embodiment parties
It is 0.01~0.02 grams per milliliter in case, and is 0.01 grams per milliliter in some specific embodiments.
According to the preparation method that the present invention is provided, wherein, the time of vibration or stirring is 1 to 5 hour in step (4), excellent
Elect as 3 hours.
According to the preparation method that the present invention is provided, wherein, the scope of regulation mixed system pH is 7~13 in step (5).
According to the preparation method that the present invention is provided, wherein, the reaction in step (5) is carried out under vibration or stirring.
In some embodiments, the reaction in step (5) is carried out in shaking table.
According to the preparation method that the present invention is provided, wherein, reaction temperature is preferably 50 DEG C in step (5).
According to the preparation method that the present invention is provided, the reaction time is 12 to 48 hours in step (5).In some embodiments
In, the reaction time is preferably 24 hours in step (5).
Advantages of the present invention includes：(1) first using starch granules as carrier, for loading Nano silver grain, obtain
Starch/silver nanoparticle compound particle；(2) the inventive method is without carrying out any surface modification, modified and function to starch granules
Change, be that this can further simplify the preparation process of supported silver nano-particle, it is easy to industrialize；(3) can efficiently control
The size and load capacity of starch particle surface Nano silver grain；(4) starch is a kind of environment-friendly natural macromolecular material, extensively
It is general to be present in the stem tuber and seed of most plants in nature, it is cheap and easy to get.
Specific embodiment
The present invention is further described in detail with reference to specific embodiment, the embodiment for being given is only for explaining
The bright present invention, rather than in order to limit the scope of the present invention.
Embodiment 1
(1) starch granules is extracted using alkaline extraction.
First, it is raw material from Grain Production of Amaranthus seed, it is clayed into power and sieved with pulverizer, is dried at 40 DEG C.Its
It is secondary, dried 50 grams of Grain Production of Amaranthus seed powders are added in 150 milliliters of n-hexanes, stir 24 hours, filtering, washing, and
It is dried to obtain the Grain Production of Amaranthus seed powder after degreasing.Finally, 2.5 mass per liter point will be added to through the Grain Production of Amaranthus seed powder of degreasing
During number is for 0.25% sodium hydroxide solution, stir 24 hours, then successively with the sieve of 70,100,200,260,300 and 400 mesh
Son filtering, filtrate is through centrifugation, and is washed with water and ethanol, through the powder sample for being dried to obtain starch granules.
Using scanning electron microscope analysis, as a result show, the average-size for obtaining starch granules is about 900 nanometers.
(2) preparation of silver ammino solution.
At room temperature, ammoniacal liquor is added dropwise to 10 milliliter 1 × 10-2In the silver nitrate aqueous solution of mol/L, solution is observed
The white precipitate of middle generation is just wholly absent, and it is 1 × 10 now to obtain concentration-2The silver ammino solution of mol/L.
(3) preparation of starch/silver nanoparticle compound particle.
At room temperature, the starch granules aqueous dispersions that 10 milliliters of concentration is 0.01 grams per milliliter are added to system in step (2)
In the silver ammino solution for obtaining, regulation system pH is 7, and vibrates mixing 3 hours.Then, 10 milliliters of PVPs are added
Ethanol solution (0.01 grams per milliliter), be warming up to 50 DEG C, and react 24 hours.Product is through centrifugation, washing and dries, and is formed sediment
Powder/silver nanoparticle compound particle.
Using starch obtained in transmission electron microscope and scanning electron microscope analysis/silver nanoparticle compound particle.As a result
It has been shown that, Nano silver grain is successfully deposited at the surface of starch granules, and its particle diameter is about 24 nanometers.
Embodiment 2
(1) starch granules is prepared using the method described in embodiment 1.
(2) silver ammino solution is prepared using the method described in embodiment 1.
(3) preparation of starch/silver nanoparticle compound particle.At room temperature, by starch that 10 milliliters of concentration is 0.01 grams per milliliter
Particle aqueous dispersion is added in step (2) in obtained silver ammino solution, and regulation system pH is 7, and vibrates mixing 3 hours.So
Afterwards, 10 milliliters of ethanol solutions of PVP (0.01 grams per milliliter) are added, 50 DEG C is warming up to, and react 24 hours.
Product is through centrifugation, washing and dries, and obtains starch/silver nanoparticle compound particle.
Using starch obtained in transmission electron microscope and scanning electron microscope analysis/silver compound particle.Result shows,
Nano silver grain is supported on the surface of starch granules, wherein, the particle diameter of Nano silver grain is 15 nanometers.
Embodiment 3
(1) starch granules is prepared using the method described in embodiment 1.
(2) silver ammino solution is prepared using the method described in embodiment 1.
(3) preparation of starch/silver nanoparticle compound particle.At room temperature, by starch that 10 milliliters of concentration is 0.01 grams per milliliter
Particle aqueous dispersion is added in step (2) in obtained silver ammino solution, and regulation system pH is 13, and vibrates mixing 3 hours.So
Afterwards, 10 milliliters of ethanol solutions of PVP (0.01 grams per milliliter) are added, 50 DEG C is warming up to, and react 24 hours.
Product is through centrifugation, washing and dries, and obtains starch/silver nanoparticle compound particle.
Using starch obtained in transmission electron microscope and scanning electron microscope analysis/silver compound particle.Result shows,
Nano silver grain is supported on the surface of starch granules, wherein, the particle diameter of Nano silver grain is 12 nanometers.
Embodiment 4
(1) starch granules is prepared using the method described in embodiment 1.
(2) silver ammino solution is prepared using the method described in embodiment 1.
(3) preparation of starch/silver nanoparticle compound particle.At room temperature, by shallow lake that 10 milliliters of concentration is 0.002 grams per milliliter
Powder particles aqueous dispersions are added in step (2) in obtained silver ammino solution, and regulation system pH is 7, and vibrates mixing 3 hours.
Then, 10 milliliters of ethanol solutions of PVP (0.01 grams per milliliter) are added, 50 DEG C are warming up to, and it is small to react 24
When.Product is through centrifugation, washing and dries, and obtains starch/silver nanoparticle compound particle.
Using starch obtained in transmission electron microscope and scanning electron microscope analysis/silver compound particle.Result shows,
Nano silver grain is supported on the surface of starch granules, wherein, the particle diameter of Nano silver grain is 46 nanometers.
Embodiment 5
(1) starch granules is prepared using the method described in embodiment 1.
(2) preparation of silver ammino solution.At room temperature, ammoniacal liquor is added dropwise to 10 milliliter 1 × 10-3The nitric acid of mol/L
In the silver-colored aqueous solution, white precipitate is produced just to be wholly absent in observation solution, it is 1 × 10 now to obtain concentration-3Mol/L
Silver ammino solution.
(3) preparation of starch/silver nanoparticle compound particle.At room temperature, by starch that 10 milliliters of concentration is 0.01 grams per milliliter
Particle aqueous dispersion is added in step (2) in obtained silver ammino solution, and regulation system pH is 7, and vibrates mixing 3 hours.So
Afterwards, 10 milliliters of ethanol solutions of PVP (0.01 grams per milliliter) are added, 50 DEG C is warming up to, and react 24 hours.
Product is through centrifugation, washing and dries, and obtains starch/silver nanoparticle compound particle.
Using starch obtained in transmission electron microscope and scanning electron microscope analysis/silver compound particle.Result shows,
Nano silver grain is supported on the surface of starch granules, wherein, the particle diameter of Nano silver grain is 10 nanometers.
Embodiment 6
(1) starch granules is prepared using the method described in embodiment 1.
(2) preparation of silver ammino solution.At room temperature, ammoniacal liquor is added dropwise to 50 milliliter of 0.02 silver nitrate of mol/L
In the aqueous solution, produce white precipitate to be just wholly absent in observation solution, now obtain the silver-colored ammonia that concentration is 0.02 mol/L
Solution.
(3) preparation of starch/silver nanoparticle compound particle.At room temperature, by starch that 50 milliliters of concentration is 0.02 grams per milliliter
Particle aqueous dispersion is added in step (2) in obtained silver ammino solution, and regulation system pH is 7, and vibrates mixing 3 hours.So
Afterwards, 50 milliliters of ethanol solutions of PVP (0.02 grams per milliliter) are added, 50 DEG C is warming up to, and react 24 hours.
Product is through centrifugation, washing and dries, and obtains starch/silver nanoparticle compound particle.
Using starch obtained in transmission electron microscope and scanning electron microscope analysis/silver compound particle.Result shows,
Nano silver grain is supported on the surface of starch granules, wherein, the particle diameter of Nano silver grain is 31 nanometers.
Claims (10)
1. a kind of preparation method of starch/silver compound particle, the described method comprises the following steps：
(1) silver-colored precursor water solution is provided；
(2) starch granules aqueous dispersions are provided；
(3) reducing agent aqueous solution is provided；
(4) the starch granules aqueous dispersions are well mixed with the silver-colored precursor water solution, and are vibrated or stirring at least 30
Minute；
(5) reducing agent aqueous solution is added to the mixture of gained in step (4), the pH of regulation system to 3~13, and
Reacted at a temperature of 25~60 DEG C, then obtain starch/silver nanoparticle compound particle solid powder through being centrifuged, washing and dry.
2. preparation method according to claim 1, wherein, the silver-colored precursor solution is selected from silver nitrate aqueous solution, three second
Hydramine silver solution, the silver acetate aqueous solution and silver ammino solution；
Preferably, in the silver-colored precursor solution silver ion concentration be 0.001~0.2 mol/L, preferably 0.001~
0.02 mol/L, more preferably 0.01~0.02 mol/L.
3. preparation method according to claim 1 and 2, wherein, the starch granules be with potato, wheat, tomato,
The root and/or stem of sweet potato or Grain Production of Amaranthus are raw material by obtained in alkaline extraction；
Preferably, the consumption of the starch granules is 1~200 times of silver-colored weight in silver-colored precursor solution, preferably 1~50 times,
More preferably 1.5~10 times, most preferably 1.75~9.5 times.
4. preparation method according to any one of claim 1 to 3, wherein, starch granules aqueous dispersions in step (2)
Concentration is 0.002~0.02 grams per milliliter, more preferably preferably 0.005~0.015 grams per milliliter, 0.01 grams per milliliter；
Preferably, the average-size of the starch granules in step (2) in starch granules aqueous dispersions is received for 100 nanometers~2000
Rice, more preferably preferably 500 nanometers~1000 nanometers, 900 nanometers.
5. preparation method according to any one of claim 1 to 4, wherein, the reducing agent is selected from trisodium citrate, boron
Sodium hydride, potassium borohydride, hydroxylamine hydrochloride, formaldehyde, hydrazine, tannic acid, sodium hypophosphite, PVP, methyl alcohol, ethanol, third
One or more in alcohol, ascorbic acid and THPC, preferably PVP；
Preferably, the consumption of the reducing agent is 0.6~600 times of silver-colored forerunner's body weight, preferably 0.6~60 times, more preferably
It is 5~10 times, and most preferably 6 times.
6. preparation method according to any one of claim 1 to 5, wherein, reductant solution is polyethylene in step (3)
The ethanol solution of base pyrrolidones；
Preferably, the concentration of the ethanol solution of PVP be 0.002~0.1 grams per milliliter, preferably 0.01~
0.1 grams per milliliter, more preferably 0.01~0.02 grams per milliliter, and most preferably 0.01 grams per milliliter.
7. preparation method according to any one of claim 1 to 6, wherein, the time of vibration or stirring is in step (4)
1 to 5 hour, preferably 3 hours.
8. preparation method according to any one of claim 1 to 7, wherein, the model of regulation mixed system pH in step (5)
It is 7~13 to enclose, preferably 7；
Preferably, the reaction in step (5) is carried out under vibration or stirring.
9. preparation method according to any one of claim 1 to 8, wherein, reaction temperature is 50 DEG C in step (5).
10. preparation method according to any one of claim 1 to 9, wherein, the reaction time is 12~48 in step (5)
Hour, preferably 24 hours.
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| CN113996801A (en) * | 2021-10-28 | 2022-02-01 | 广东省科学院微生物研究所(广东省微生物分析检测中心) | Method for preparing nano-silver based on red amaranth extracting solution |
| EP4088838A1 (en) * | 2021-05-12 | 2022-11-16 | Heraeus Deutschland GmbH & Co. KG | Method for the preparation of silver powder |
| CN116387692A (en) * | 2023-05-31 | 2023-07-04 | 宁波齐云新材料技术有限公司 | Lithium battery pack intelligent heat dissipation control system and control method thereof |
| CN116589636A (en) * | 2023-07-19 | 2023-08-15 | 上海宇昂水性新材料科技股份有限公司 | Silver nanowire end capping agent and preparation method and application thereof |
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Application publication date: 20170531 |