CN104999072B - A kind of redispersible nano silver wire mixture and preparation method thereof - Google Patents
A kind of redispersible nano silver wire mixture and preparation method thereof Download PDFInfo
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Abstract
This case discloses a kind of redispersible nano silver wire mixture and preparation method thereof, including nano silver wire and dispersant, wherein dispersant includes organo-silicon compound, the high-molecular compound containing ether or carboxyl or amino or at least one of carboxy derivatives or aminoderivative group, containing ether or carboxyl or amino or the long-chain macromolecule of at least one of carboxy derivatives or aminoderivative group or its combination.This case to nano silver wire by carrying out surface modification, the surface for not only significantly reducing nano silver wire can, the purpose of hydrophobic/hydrophilic is realized with this, further improve the reunion situation of nano silver wire in the solution, these nano silver wires can be more made to the solid mixt state such as powder or paste, both the long-term preservation to these nano silver wires had been realized, may be such that it has splendid redispersibility energy in organic solvent again.
Description
Technical field
The present invention relates to a kind of modification of the surface of nano silver wire, and in particular to a kind of redispersible nano silver wire mixture
And preparation method thereof.
Background technology
Nano silver wire is a kind of material at least one-dimensional size in nanometer range, and this material has excellent lead
Electrical property, antibiotic property and catalytic, with extensive potential application, especially nano silver wire, they can be used for preparing flexibility thoroughly
Prescribed electrode is used to replace ITO electro-conductive glass, and the nesa coating of preparation has higher electric conductivity and transparency, and is adapted to big
The volume to volume production of scale.
At present, commercially available nano silver wire majority occurs in the form of dispersion liquid, and concentration is very low, and through after a period of time
Precipitation can be produced and reunited, be unfavorable for storage and volume production is used, its reason can be higher mainly due to the surface of nano silver wire,
Reunion easily is produced, it is necessary to be dispersed in specific solvent, and is extremely difficult to high concentration, and due to there is larger surface
Can, it is difficult to matched with hydrophobic medium.
Prior art is mostly focused on the modification of micro nanometer silver material, and primarily directed to the processing of powder, and silver is received
Rice noodles have more specifically property compared to silver-colored microballoon, and surface modified about nano silver wire there is no relevant this respect problem
Report.
The content of the invention
For the defect of prior art, it is contemplated that surface energy and can be improved by the surface for reducing nano silver wire, reach
To nano silver wire and the purpose of solvent interface compatibility is improved, these nano materials are enable to be preserved for a long time in solid form
It is not susceptible to reunite or precipitates, it is possible to which there is good weight dispersiveness in organic media.
Technical scheme is summarized as follows：
A kind of redispersible nano silver wire mixture, including：
Nano silver wire；The diameter range of the nano silver wire is 30~120nm；Length range is 10~200 μm.
Dispersant, the dispersant is selected from organo-silicon compound, contains ether or carboxyl or amino or carboxy derivatives or ammonia
The high-molecular compound of at least one of radical derivative group, spread out containing ether or carboxyl or amino or carboxy derivatives or amino
The long-chain macromolecule of at least one of biology group or its combination；
Wherein, the draw ratio of the nano silver wire is 200~1000.
Preferably, described redispersible nano silver wire mixture, wherein, using parts by weight to count, the silver nanoparticle
100 parts of line, 1~100 part of the dispersant.
Preferably, described redispersible nano silver wire mixture, wherein, the organo-silicon compound are selected from silane
Coupling agent, fluorine containing silane, siloxanes, silicon nitrilo compound or its combination.
Preferably, described redispersible nano silver wire mixture, wherein, the silane coupler is γ-methyl
Acryloxypropyl trimethoxy silane, N- (β-aminoethyl)-γ-aminopropyltriethoxy dimethoxysilane, γ-(2,3- rings
Oxygen propoxyl group) one kind in propyl trimethoxy silicane, fluorine containing silane or HMDO.
Preferably, described redispersible nano silver wire mixture, wherein, the high-molecular compound is polyethylene
Pyrrolidones or polyethylene glycol.
Preferably, described redispersible nano silver wire mixture, wherein, the long-chain macromolecule is selected from fat
One kind in acid, stearic acid, oleic acid or triethanolamine oleate.
A kind of preparation method of redispersible nano silver wire mixture, including：
Step 1) nano silver wire of 100 parts by weight is suspended in dispersion liquid, the dispersion liquid be selected from ethanol, ethylene glycol,
Propane diols, n-butanol, isopropanol, glycerine, n-hexyl alcohol or its combination；
Step 2) dispersant of 1~100 parts by weight of addition into dispersion liquid, stir, obtain mixed liquor；It is described scattered
Agent is selected from organo-silicon compound, contains ether or carboxyl or amino or at least one of carboxy derivatives or aminoderivative group
High-molecular compound, the length containing ether or carboxyl or amino or at least one of carboxy derivatives or aminoderivative group
Chain macromolecular or its combination；
Step 3) by vacuum distillation or by precipitating, filtering, centrifuge out nano silver wire.
Preferably, the preparation method of described redispersible nano silver wire mixture, wherein, the organosilicon compound
Thing be γ-methacryloxypropyl trimethoxy silane, N- (β-aminoethyl)-γ-aminopropyltriethoxy dimethoxysilane,
One kind in γ-(2,3- glycidoxy) propyl trimethoxy silicane, fluorine containing silane or HMDO；The high score
Sub- compound is polyvinylpyrrolidone or polyethylene glycol.
Preferably, the preparation method of described redispersible nano silver wire mixture, wherein, the nano silver wire
Draw ratio is 200~1000.
Preferably, the preparation method of described redispersible nano silver wire mixture, wherein, when the producing high-molecular
When compound is polyvinylpyrrolidone, the K values of the polyvinylpyrrolidone are 10~90；The degree of polymerization of the polyethylene glycol is
200~4000.
The beneficial effects of the invention are as follows：Surface modification is carried out to nano silver wire by three kinds of methods, not only significantly reduced
The surface energy of these three nano silver wires, the purpose of hydrophobic/hydrophilic is realized with this, the group of nano silver wire in the solution is further improved
Poly- situation, more these nano silver wires can be made to the solid mixt state such as powder or paste, both realized and these silver had been received
The long-term preservation of rice noodles, may be such that it has splendid redispersibility energy in organic solvent again.
Embodiment
With reference to embodiment, the present invention is described in further detail, to make those skilled in the art with reference to specification
Word can be implemented according to this.
This case proposes the redispersible nano silver wire mixture of an embodiment, including：
Nano silver wire can be that suspended state can also be paste or solid state in the technical scheme before processing through this case.
And be emphasized that the nano silver wire used in this case does not have particular/special requirement to its purity, it is required in the prior art using pure
Degree ＞ 99% nano silver wire makees raw material, and this case is without doing concrete restriction to purity, that is to say, that this case can use low pure
The nano silver wire of degree does raw material, and the technical scheme of this case also has purification function in itself, therefore can be big using the technical program
Big reduction production cost.
Dispersant, selected from organo-silicon compound, contains ether or carboxyl or amino or carboxy derivatives or aminoderivative
At least one of the high-molecular compound of group, containing in ether or carboxyl or amino or carboxy derivatives or aminoderivative extremely
A kind of long-chain macromolecule of few group or its combination.Organo-silicon compound are selected from silane coupler, fluorine containing silane, siloxanes, silicon
Nitrilo compound or its combination.
Wherein, the ratio of the draw ratio of nano silver wire, i.e. length/diameter must be limited, and its value is preferably 200~1000.It is real
Issue after examination and approval now, the effect that the draw ratio of nano silver wire is modified on surface plays very important influence, inappropriate nano silver wire
Draw ratio, can cause dispersant to deviate ideal effect to the surface modification of nano silver wire, cause the nano silver wire finally given to mix
The redisperse hydraulic performance decline of compound, after nano silver wire mixture redisperse suspends, it has occurred the probability of sedimentation reunion again
Rise.If the draw ratio of nano silver wire is less than 200, dispersant is caused to weaken the covering property of nano silver wire so that part silver
It is exposed in suspension so that this barish silver wire is reunited；If the draw ratio of nano silver wire is more than 1000, due to
The length of nano wire is long so that winding friction easily occurs for the nano silver wire after modification, so that the dispersant of cladding can be influenceed
Stability, after breakage occurs for the material that nanowire surface is coated, nano wire is reunited at once, so as to cause nano wire
Suspension fails.As optimal case, the draw ratio of nano silver wire is can be controlled between 500~600, within this range, can be made
Obtain nano silver wire mixture and obtain the stabilization after most permanent period of storage, most quick dispersion rate and optimal redisperse
Property.
As the another embodiment of this case, wherein, the addition of nano silver wire is 100 parts by weight, and the addition of dispersant is 1
~100 parts by weight.Experiment is found, under this ratio, and the redisperse effect of obtained nano silver wire mixture is best, through multiple
Experiment, does not find to dissipate the example of reunion after redisperse.
As the another preferred embodiment of this case, wherein, silane coupler is γ-methacryloxypropyl front three
TMOS, N- (β-aminoethyl)-γ-aminopropyltriethoxy dimethoxysilane, γ-(2,3- glycidoxy) propyl group trimethoxy
One kind in base silane, fluorine containing silane or HMDO.Experiment is found, when several silane coupled containing this in dispersant
During agent, gained nano silver wire mixture has preferably redisperse effect, can meet long-term shelf appeal.And in this 5 kinds of silane
In coupling agent, γ-methacryloxypropyl trimethoxy silane, N- (β-aminoethyl)-γ-aminopropyltriethoxy diformazan are belonged to again
These three best results of TMOS, γ-(2,3- glycidoxy) propyl trimethoxy silicane.
If when containing polyvinylpyrrolidone (PVP) in dispersant, being preferably defined to its K value, when K values for 10~
When 90, nano silver wire mixture can be made to obtain quick redisperse speed, and the appropriate viscosity body brought by K values
System, not only causes the redisperse excellent of nano silver wire mixture, and results in and stablize permanent storage time.If K
Value is less than 10, then can reduce parcel effects of the PVP to nano silver wire, add the reunion wind after nano silver wire mixture redisperse
Danger；If K values are more than 90, because PVP viscosity is too high, cause the redisperse speed of nano silver wire mixture in organic solvent
It is slack-off, or even can not disperse again, cause nano silver wire mixture to fail.
This case proposes the preparation method of this redispersible nano silver wire mixture simultaneously, including：
Step 1) nano silver wire of 100 parts by weight is suspended in dispersion liquid, dispersion liquid is selected from ethanol, ethylene glycol, the third two
Alcohol, n-butanol, isopropanol, glycerine or its combination；
Step 2) dispersant of 10~20 parts by weight of addition into dispersion liquid, stir, obtain mixed liquor；Dispersant is selected
Height from organo-silicon compound, containing ether or carboxyl or amino or at least one of carboxy derivatives or aminoderivative group
Molecular compound, the long-chain containing ether or carboxyl or amino or at least one of carboxy derivatives or aminoderivative group are big
Molecule or its combination；
Step 3) by precipitating, filtering, centrifuge or isolate nano silver wire by vacuum distillation.In 110 DEG C, -0.05
Vacuum distillation is carried out to mixed liquor until drying under~-0.1MPa, nano silver wire mixture is obtained.
Embodiment 1
The nano silver wire that the draw ratio for being 10mg by gross weight is 200 is suspended in 100ml ethanol；Added into ethanol
1mg γ-methacryloxypropyl trimethoxy silane, stirs, obtains mixed liquor；Then at 45~55 DEG C ,-
Vacuum distillation is carried out to mixed liquor until drying under 0.05~-0.06MPa, the nano silver wire mixture of solid-like is obtained.Storage
After 10 days, nano silver wire mixture obtained above is added in 100ml ethanol or isopropanol, ultrasonic agitation 1 hour is obtained
Again scattered nano silver wire, measured its stabilization time more than 3 months.
Embodiment 2
The nano silver wire that the draw ratio for being 10mg by gross weight is 1000 is suspended in 100ml ethanol；Added into ethanol
1mg γ-methacryloxypropyl trimethoxy silane, stirs, obtains mixed liquor；Then at 45~55 DEG C ,-
Vacuum distillation is carried out to mixed liquor until drying under 0.05~-0.06MPa, the nano silver wire mixture of solid-like is obtained.Storage
After a few days, nano silver wire mixture obtained above is added in 100ml ethanol, ultrasonic agitation half an hour, divided again
Scattered nano silver wire, its stabilization time is more than 3 months.
Embodiment 3
The nano silver wire that the draw ratio for being 20mg by gross weight is 500 is suspended in 100ml ethylene glycol；Add into ethylene glycol
Plus 1mg N- (β-aminoethyl)-γ-aminopropyltriethoxy dimethoxysilane, stir, obtain mixed liquor；Then 45~
55 DEG C, vacuum distillation is carried out to mixed liquor until drying under -0.05~-0.06MPa, the nano silver wire mixing of solid-like is obtained
Thing.Store after a few days, nano silver wire mixture obtained above is added in 100ml isopropanols, ultrasonic agitation half an hour, obtained
To again scattered nano silver wire, its stabilization time is more than 3 months.
Embodiment 4
The nano silver wire that the draw ratio for being 20mg by gross weight is 600 is suspended in 100ml propane diols, is added into dispersion liquid
Plus 1mg γ-(2,3- glycidoxy) propyl trimethoxy silicane, stir, obtain mixed liquor；Then 45~55
DEG C, vacuum distillation is carried out to mixed liquor until drying under -0.05~-0.06MPa, solid-like nano silver wire mixture is obtained.Storage
Deposit after a few days, nano silver wire mixture obtained above is added in 100ml n-butanols, ultrasonic agitation half an hour, obtain weight
The nano silver wire newly disperseed, its stabilization time is more than 3 months.
Embodiment 5
The nano silver wire that the draw ratio for being 10mg by gross weight is 200 is suspended in 100ml n-butanols；Add into n-butanol
Plus 1mg triethoxy -1H, 1H, 2H, 2H- perfluoro decyl silane, stir, obtain mixed liquor；Then at 45~55 DEG C ,-
Vacuum distillation is carried out to mixed liquor until drying under 0.05~-0.06MPa, the nano silver wire mixture of solid-like is obtained.Storage
After a few days, nano silver wire mixture obtained above is added in 100ml n-hexyl alcohols, ultrasonic agitation 1 hour is divided again
Scattered nano silver wire, its stabilization time is more than 2 months.
Embodiment 6
The nano silver wire that the draw ratio for being 10mg by gross weight is 1000 is suspended in 100ml isopropanols, into isopropanol
1mg HMDO is added, stirs, obtains mixed liquor；Then at 45~55 DEG C, under -0.05~-0.06MPa
Vacuum distillation is carried out to mixed liquor until drying, nano silver wire mixture is obtained.Store after a few days, by silver nanoparticle obtained above
Line mixture is added in 100ml n-butanols, ultrasonic agitation half an hour, the nano silver wire disperseed again, its stabilization time
More than 2 months.
Embodiment 7
The nano silver wire that the draw ratio for being 10mg by gross weight is 300 is suspended in 100ml glycerine, is added into glycerine
Plus 10mg polyvinylpyrrolidone (K value=30), stir, obtain mixed liquor；Then at 45~55 DEG C, -0.05~-
Vacuum distillation is carried out to mixed liquor until drying under 0.06MPa, nano silver wire mixture is obtained.Store after a few days, obtained above-mentioned
To nano silver wire mixture be added in 100ml isopropanols, ultrasonic agitation half an hour, the nano silver wire disperseed again,
Its stabilization time is more than 3 months.
Embodiment 8
The nano silver wire that the draw ratio for being 10mg by gross weight is 400 is suspended in 100ml ethanol, is added into ethanol
20mg polyvinylpyrrolidone (K value=90), stirs, obtains mixed liquor；Then at 45~55 DEG C, -0.05~-
Vacuum distillation is carried out to mixed liquor until drying under 0.06MPa, nano silver wire mixture is obtained.Store after a few days, obtained above-mentioned
To nano silver wire mixture be added in 100ml n-butanols, ultrasonic agitation half an hour, the nano silver wire disperseed again,
Its stabilization time is more than 3 months.
Embodiment 9
The nano silver wire that the draw ratio for being 1mg by gross weight is 400 is suspended in 100ml ethylene glycol, is added into ethylene glycol
Plus 10mg polyethylene glycol (degree of polymerization is 4000), stir, obtain mixed liquor；Then at 100~110 DEG C, -0.095~-
Vacuum distillation is carried out to mixed liquor under 0.1MPa until pasty state drying, obtains nano silver wire mixture.Store after a few days, will be above-mentioned
Obtained nano silver wire mixture is added in 100ml ethanol, ultrasonic agitation 1 hour, the nano silver wire disperseed again, its
Stabilization time is more than 1 month.
Embodiment 10
The nano silver wire that the draw ratio for being 10mg by gross weight is 800 is suspended in 100ml propane diols, is added into propane diols
Plus 20mg oleic acid, stir, obtain mixed liquor；Then at 100~110 DEG C, mixed liquor is entered under -0.095~-0.1MPa
Row vacuum distillation is until pasty state drying, obtains nano silver wire mixture.Store after a few days, nano silver wire obtained above is mixed
Thing is added in 100ml ethanol, ultrasonic agitation half an hour, the nano silver wire disperseed again, and its stabilization time is more than 3
Month.
Embodiment 11
The nano silver wire that the draw ratio for being 10mg by gross weight is 900 is suspended in 100ml n-butanols, is added into n-butanol
Plus 10mg triethanolamine oleate, stir, obtain mixed liquor；It is right under -0.095~-0.1MPa then at 100~110 DEG C
Mixed liquor carries out vacuum distillation until drying, and obtains nano silver wire mixture.Store after a few days, by nano silver wire obtained above
Mixture is added in 100ml isopropanols, and ultrasonic agitation half an hour, the nano silver wire disperseed again, its stabilization time is big
In 3 months.
Embodiment 12
The nano silver wire that the draw ratio for being 1mg by gross weight is 700 is suspended in 100ml ethylene glycol, is added into ethylene glycol
Plus 10mg stearic acid, stir, obtain mixed liquor；Then at 100~110 DEG C, to mixed liquor under -0.095~-0.1MPa
Vacuum distillation is carried out until pasty state drying, obtains nano silver wire mixture.Store after a few days, nano silver wire obtained above is mixed
Compound is added in 100ml n-butanols, ultrasonic agitation 1 hour, the nano silver wire disperseed again, and its stabilization time is more than 1
Individual month.
Comparative example 1
The 100ml absolute ethyl alcohol suspension for the nano silver wire for being 200 to the draw ratio for being 10mg containing weight, adds 1mg
γ-methacryloxypropyl trimethoxy silane, stir, obtain mixed liquor；Then in 45~55 DEG C, -0.05
Vacuum distillation is carried out to mixed liquor until drying under~-0.06MPa, the nano silver wire mixture of solid-like is obtained, it is measured and consolidates
The period of storage of body is to remain within 2 months through ultrasonic disperse in the isopropanol with former ratio.Unmodified above-mentioned nano silver wire is hanged
Supernatant liquid is stood, and is measured its stabilization time for reunion takes place after 20 hours, 20 hours, is all reunited after 2 days.
Comparative example 2
The 100ml absolute ethyl alcohol suspension for the nano silver wire for being 1000 to the draw ratio for being 10mg containing weight；Add 2mg
γ-methacryloxypropyl trimethoxy silane, stir, obtain mixed liquor；Then in 45~55 DEG C, -0.05
Vacuum distillation is carried out to mixed liquor until drying under~-0.06MPa, the nano silver wire mixture of solid-like is obtained, it is measured and consolidates
The period of storage of body was remained to through ultrasonic disperse more than 2 months in the n-butanol with former ratio.By unmodified above-mentioned nano silver wire
Suspension, which is stood, measures its stabilization time for reunion takes place after 3 hours, 3 hours, all reunites after 10 hours.
Comparative example 3
The nano silver wire that the draw ratio for being 10mg by gross weight is 300 is suspended in 100ml ethanol, and addition 10mg's is poly-
Vinylpyrrolidone (K values are 30), stirs, obtains mixed liquor；It is right under -0.05~-0.06MPa then at 45~55 DEG C
Mixed liquor carry out vacuum distillation until dry, obtain nano silver wire mixture, its storage time more than 2 months after remain to through ultrasound
After be dispersed in water, by unmodified above-mentioned nano silver wire suspension ultrasonic agitation 1 hour, its stabilization time was after 2 days, 2 days
Reunion takes place, all reunites after 5 days.
Comparative example 4
The nano silver wire that the draw ratio for being 10mg by gross weight is 400 is suspended in 100ml ethanol, is added into ethanol
10mg polyvinylpyrrolidone (K values are 90), stirs, obtains mixed liquor；Then at 45~55 DEG C, -0.05~-
Vacuum distillation is carried out to mixed liquor until drying under 0.06MPa, nano silver wire mixture is obtained, its storage time was more than 3 months
After remain to be dispersed in water after ultrasound, by unmodified above-mentioned nano silver wire suspension ultrasonic agitation 1 hour, its stabilization time
For reunion takes place after 2 days, 2 days, all reunite after 5 days.
Although embodiment of the present invention is disclosed as above, it is not restricted in specification and embodiment listed
With it can be applied to various suitable the field of the invention completely, can be easily for those skilled in the art
Other modification is realized, therefore under the universal limited without departing substantially from claim and equivalency range, the present invention is not limited
In specific details and shown here embodiment.
Claims (2)
1. a kind of redispersible nano silver wire mixture, including：
Nano silver wire；
Dispersant, the dispersant is selected from organo-silicon compound, spread out containing ether or carboxyl or amino or carboxy derivatives or amino
The high-molecular compound of at least one of biology group, contain ether or carboxyl or amino or carboxy derivatives or aminoderivative
At least one of the long-chain macromolecule of group or its combination；
Wherein, the draw ratio of the nano silver wire is 200~1000；
Using parts by weight to count, 100 parts of the nano silver wire, 1~100 part of the dispersant；
The organo-silicon compound are selected from silane coupler, fluorine containing silane, siloxanes, silicon nitrilo compound or its combination；
The silane coupler is γ-methacryloxypropyl trimethoxy silane, N- (β-aminoethyl)-γ-aminopropyl
Methyl dimethoxysilane, γ-(2,3- glycidoxies) propyl trimethoxy silicane, fluorine containing silane or HMDO
In one kind；
The high-molecular compound is polyvinylpyrrolidone or polyethylene glycol；
The one kind of the long-chain macromolecule in aliphatic acid, stearic acid, oleic acid or triethanolamine oleate.
2. a kind of preparation method of redispersible nano silver wire mixture, including：
Step 1) nano silver wire of 100 parts by weight is suspended in dispersion liquid, the dispersion liquid is selected from ethanol, ethylene glycol, the third two
Alcohol, n-butanol, isopropanol, glycerine, n-hexyl alcohol or its combination；
Step 2) dispersant of 1~100 parts by weight of addition into dispersion liquid, stir, obtain mixed liquor；The dispersant choosing
Height from organo-silicon compound, containing ether or carboxyl or amino or at least one of carboxy derivatives or aminoderivative group
Molecular compound, the long-chain containing ether or carboxyl or amino or at least one of carboxy derivatives or aminoderivative group are big
Molecule or its combination；
Step 3) by vacuum distillation or by precipitating, filtering, centrifuge out nano silver wire；
The organo-silicon compound are γ-methacryloxypropyl trimethoxy silane, N- (β-aminoethyl)-γ-ammonia third
Ylmethyl dimethoxysilane, γ-(2,3- glycidoxies) propyl trimethoxy silicane, fluorine containing silane or silica of hexamethyl two
One kind in alkane；The high-molecular compound is polyvinylpyrrolidone or polyethylene glycol；
The draw ratio of the nano silver wire is 200~1000；
When the high-molecular compound is polyvinylpyrrolidone, the K values of the polyvinylpyrrolidone are 10~90；It is described
The degree of polymerization of polyethylene glycol is 200~4000.
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| CN102744417A (en) * | 2011-06-16 | 2012-10-24 | 浙江科创新材料科技有限公司 | Method for preparing nano-silver wire with high length-diameter ratio |
| CN103100724A (en) * | 2013-02-21 | 2013-05-15 | 中国科学院深圳先进技术研究院 | Preparation method of silver nanowires |
| CN103614090A (en) * | 2013-12-06 | 2014-03-05 | 苏州贤聚科技有限公司 | Antistatic pressure-sensitive adhesive protective film and preparation method thereof |
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