CN109848433A - A kind of fast and convenient method for preparing dendritic nano-silver - Google Patents
A kind of fast and convenient method for preparing dendritic nano-silver Download PDFInfo
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- CN109848433A CN109848433A CN201711242397.5A CN201711242397A CN109848433A CN 109848433 A CN109848433 A CN 109848433A CN 201711242397 A CN201711242397 A CN 201711242397A CN 109848433 A CN109848433 A CN 109848433A
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Abstract
The invention belongs to the field of chemical synthesis, disclose a kind of fast and convenient method for preparing dendritic nano-silver.Method includes the following steps: (1) is mixed polyvinylpyrrolidone, silver nitrate and sodium chloride, it is dissolved in ethylene glycol, is uniformly mixed；(2) mixed liquor obtained after being uniformly mixed in step (1) carries out segmentally heating reaction, after reaction purifies gained reaction solution up to dendritic nano-silver.Dendritic nano-silver is prepared using this method, avoids the preparation of relatively complicated complexity and purifying technique in traditional preparation methods, it is relatively low to the requirement for preparing environment, it can be convenient and rapidly prepare dendritic nano-silver.
Description
Technical field
The invention belongs to the field of chemical synthesis, in particular to a kind of fast and convenient method for preparing dendritic nano-silver.
Background technique
Nano silver material is applied to many electronic materials, electronics because of its unique electrical and optical performance in recent years
In component equipment, wherein nano-Ag particles are applied in anti-biotic material and conductive adhesive more, and nano-silver thread is applied more
In transparent conductive film, and dendritic nano-silver both has what nano-silver thread was mutually put up a bridge as a kind of monodimension nanometer material
Characteristic can be improved connected ratio of the nano material when being conductively connected, avoid nano-silver thread but also with unique topological structure
The interleaved mode by adjusting silver wire is needed to improve the operating procedure of conductivity in film forming, this feature makes it in conduction
Application on material has biggish advantage.The report of the current existing synthetic method about dendritic nano-silver mainly has electricity
Chemical method and wet chemistry method, but both methods or be to have more complicated operating procedure or harsh synthesis condition,
Complex in subsequent purification technique, these conditions all significantly limit dendritic nano-silver on more on a large scale
Preparation, the synthesis scale of dendritic nano-silver are limited in laboratory level always.Therefore, develop one kind has on synthesis technology
Easy quick feature, and the preparation method of not extremely complex subsequent purification steps is just particularly important.
Summary of the invention
In order to overcome the shortcomings and deficiencies of the prior art described above, the primary purpose of the present invention is that providing a kind of fast and convenient
The method for preparing dendritic nano-silver.
The purpose of the present invention is realized by following proposal:
A kind of fast and convenient method for preparing dendritic nano-silver, uses polyvinylpyrrolidone as dispersing agent, nitric acid
Silver is used as presoma, and ethylene glycol is divided into following steps as nucleating agent, specific preparation method as solvent, sodium chloride:
(1) polyvinylpyrrolidone, silver nitrate and sodium chloride are mixed, is dissolved in ethylene glycol, is uniformly mixed
Obtain mixed liquor；
(2) mixed liquor obtained after being uniformly mixed in step (1) carries out segmentally heating reaction, after reaction will
Gained reaction solution purifies up to dendritic nano-silver.
The molecular weight of polyvinylpyrrolidone described in step (1) can be 3500,8000,40000 or 58000.
According to the difference of the molecular weight of polyvinylpyrrolidone, the ratio of silver nitrate, sodium chloride and ethylene glycol is added in selection:
When polyvinylpyrrolidonemolecules molecules amount is 3500, the polyvinylpyrrolidone of addition and the weight ratio of silver nitrate are 4:1；When poly-
When vinylpyrrolidone molecular weight is 8000, the polyvinylpyrrolidone of addition and the weight ratio of silver nitrate are 3:1；Work as polyethylene
When pyrrolidone molecule amount is 40000, the polyvinylpyrrolidone of addition and the weight ratio of silver nitrate are 1.8:1；Work as polyethylene
When pyrrolidone molecule amount is 58000, the polyvinylpyrrolidone of addition and the weight ratio of silver nitrate are 1.2:1；
The additive amount of sodium chloride and the weight ratio of silver nitrate are between 1:300 to 1:900；The additive amount of ethylene glycol is nitric acid
100 times of silver-colored weight.
Segmentally heating described in step (2), which is reacted, refers to heating reaction in two stages, and first stage heating reaction, which refers to, to be added
Heat is to 40~100 DEG C of 0.5~2h of reaction, and heating is reacted into second stage heating after reaction for first stage heating, and second
Stepwise heating reaction, which refers to, is heated to 120~160 DEG C of 1~5h of reaction；
Preferably, first stage heating reaction, which refers to, is heated to 50~70 DEG C of reaction 1h；Second stage heating reaction refers to heating
To 120~130 DEG C of reaction 2h.
Purifying described in step (2), which refers to, is cooled to room temperature gained reaction solution, and addition is twice in the third of reaction solution volume
Ketone stands 10min, all removes supernatant liquor after all nano silver products are all deposited in bottom, 1wt% is then added
Aqueous povidone solution scatters precipitating, and adding acetone settles nano silver, after repeating three times this settling operations, institute
Obtaining bottom precipitation is dendritic nano-silver.Dendritic nano-silver is fabricated to dispersion liquid using ethanol solution for using.
The present invention compared with the existing technology, have the following advantages and the utility model has the advantages that
Method of the invention prepares dendritic nano-silver, avoid in traditional preparation methods the preparation of relatively complicated complexity and
Purifying technique, it is relatively low to the requirement for preparing environment, it can be convenient and rapidly prepare dendritic nano-silver.
Detailed description of the invention
Fig. 1 is the TEM figure of product prepared by embodiment 1；
Fig. 2 is the TEM figure of product prepared by embodiment 2；
Fig. 3 is the TEM figure of product prepared by embodiment 3；
Fig. 4 is the TEM figure of product prepared by embodiment 4；
Specific embodiment
Below with reference to embodiment and attached drawing, the present invention is described in further detail, but embodiments of the present invention are unlimited
In this.
Agents useful for same can routinely be bought unless otherwise specified from market in embodiment.
Embodiment 1
By 1g silver nitrate, the polyvinylpyrrolidone that 4g molecular weight is 3500, the sodium chloride of 3mg and the ethylene glycol of 100g add
Enter into the two mouth flask of 200mL, 90 DEG C of agitating and heatings are reacted 1 hour, are then reacted 3 hours at 130 DEG C again, and reaction is stopped
Afterwards, it after reaction solution natural cooling, is settled using acetone, reuses the aqueous povidone solution dilution of 1% weight ratio
Three times, last spent glycol prepared composition dispersion liquid uses.
Embodiment 2
By 10g silver nitrate, the polyvinylpyrrolidone that 30g molecular weight is 8000, the sodium chloride of 20mg and the second two of 1000g
Alcohol is added in the two mouth flask of 2L, and 80 DEG C of agitating and heatings are reacted 1.5 hours, are then reacted 2.5 hours at 120 DEG C again, is stopped
It after reaction, after reaction solution natural cooling, is settled using acetone, reuses the aqueous povidone solution of 1% weight ratio
Dilution three times, last spent glycol prepared composition dispersion liquid use.
Embodiment 3
By 4g silver nitrate, the polyvinylpyrrolidone that 7.2g molecular weight is 40000, the sodium chloride of 10mg and the second two of 400g
Alcohol is added in the two mouth flask of 1L, and 100 DEG C of agitating and heatings are reacted 0.5 hour, are then reacted 2 hours at 150 DEG C again, is stopped anti-
Ying Hou is settled after reaction solution natural cooling using acetone, and the aqueous povidone solution for reusing 1% weight ratio is dilute
It releases three times, last spent glycol prepared composition dispersion liquid uses.
Embodiment 4
By 2g silver nitrate, the polyvinylpyrrolidone that 2.4g molecular weight is 58000, the sodium chloride of 4mg and the second two of 200g
Alcohol is added in the two mouth flask of 500mL, and 60 DEG C of agitating and heatings are reacted 1 hour, are then reacted 2 hours at 120 DEG C again, is stopped anti-
Ying Hou is settled after reaction solution natural cooling using acetone, and the aqueous povidone solution for reusing 1% weight ratio is dilute
It releases three times, last spent glycol prepared composition dispersion liquid uses.
The dendritic nano-silver dispersant liquid drop prepared in Examples 1 to 4 is added in carbon to support to be prepared into sample on film copper mesh
TEM test is carried out, as a result as shown in figures 1-4, wherein Fig. 1,2,3,4 respectively correspond the product prepared for embodiment 1,2,3,4
TEM figure.As can be seen from the figure the present invention is successfully prepared dendritic nano-silver.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any changes, modifications, substitutions, combinations, simplifications made without departing from the spirit and principles of the present invention,
It should be equivalent substitute mode, be included within the scope of the present invention.
Claims (7)
1. a kind of fast and convenient method for preparing dendritic nano-silver, it is characterised in that use polyvinylpyrrolidone as dispersion
Agent, silver nitrate as presoma, ethylene glycol as solvent, sodium chloride as nucleating agent, specifically includes the following steps:
(1) polyvinylpyrrolidone, silver nitrate and sodium chloride are mixed, is dissolved in ethylene glycol, what is be uniformly mixed is mixed
Close liquid；
(2) mixed liquor obtained after being uniformly mixed in step (1) carries out segmentally heating reaction, after reaction by gained
Reaction solution purifies up to dendritic nano-silver.
2. the fast and convenient method for preparing dendritic nano-silver according to claim 1, it is characterised in that:
The molecular weight of polyvinylpyrrolidone described in step (1) is 3500,8000,40000 or 58000.
3. the fast and convenient method for preparing dendritic nano-silver according to claim 2, it is characterised in that:
When polyvinylpyrrolidonemolecules molecules amount is 3500, the polyvinylpyrrolidone of addition and the weight ratio of silver nitrate are 4:1；
When polyvinylpyrrolidonemolecules molecules amount is 8000, the polyvinylpyrrolidone of addition and the weight ratio of silver nitrate are 3:1；When poly-
When vinylpyrrolidone molecular weight is 40000, the polyvinylpyrrolidone of addition and the weight ratio of silver nitrate are 1.8:1；When poly-
When vinylpyrrolidone molecular weight is 58000, the polyvinylpyrrolidone of addition and the weight ratio of silver nitrate are 1.2:1；
The additive amount of sodium chloride and the weight ratio of silver nitrate are between 1:300 to 1:900；The additive amount of ethylene glycol is silver nitrate weight
100 times of amount.
4. the fast and convenient method for preparing dendritic nano-silver according to claim 1, it is characterised in that:
The reaction of segmentally heating described in step (2) refers to heating reaction in two stages, and first stage heating reaction, which refers to, to be heated to
40~100 DEG C of 0.5~2h of reaction, heating enters second stage heating reaction, second stage after reaction for first stage heating
Heating reaction, which refers to, is heated to 120~160 DEG C of 1~5h of reaction.
5. the fast and convenient method for preparing dendritic nano-silver according to claim 4, it is characterised in that:
The heating reaction of first stage described in step (2), which refers to, is heated to 50~70 DEG C of reaction 1h.
6. the fast and convenient method for preparing dendritic nano-silver according to claim 4, it is characterised in that:
The heating reaction of second stage described in step (2), which refers to, is heated to 120~130 DEG C of reaction 2h.
7. the fast and convenient method for preparing dendritic nano-silver according to claim 1, it is characterised in that:
Purifying described in step (2), which refers to, is cooled to room temperature gained reaction solution, and the acetone that addition is twice in reaction solution volume is quiet
10min is set, all removes supernatant liquor after all nano silver products are all deposited in bottom, the poly- second of 1wt% is then added
Alkene pyrrolidone aqueous solution scatters precipitating, and adding acetone settles nano silver, after repeating three times this settling operations, gained bottom
Portion's precipitating is dendritic nano-silver.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115446325A (en) * | 2022-09-21 | 2022-12-09 | 广东石油化工学院 | Metal powder with multi-level branch structure and preparation method thereof |
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| CN101579746A (en) * | 2008-05-13 | 2009-11-18 | 中国科学院理化技术研究所 | Method for preparing micron-grade superfine silver powder with shape of pinecone, flower or tree |
| CN101811196A (en) * | 2010-05-11 | 2010-08-25 | 中国乐凯胶片集团公司 | Method for preparing dendritic micron silver powder |
| US20120297927A1 (en) * | 2011-05-23 | 2012-11-29 | Carestream Health, Inc. | Branched nanowire preparation methods, compositions, and articles |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115446325A (en) * | 2022-09-21 | 2022-12-09 | 广东石油化工学院 | Metal powder with multi-level branch structure and preparation method thereof |
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Application publication date: 20190607 |