CN109111714A - Silver nanowires modified fullerenes micro/nano-fibre, preparation method and applications - Google Patents
Silver nanowires modified fullerenes micro/nano-fibre, preparation method and applications Download PDFInfo
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- CN109111714A CN109111714A CN201810829164.3A CN201810829164A CN109111714A CN 109111714 A CN109111714 A CN 109111714A CN 201810829164 A CN201810829164 A CN 201810829164A CN 109111714 A CN109111714 A CN 109111714A
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L69/00—Compositions of polycarbonates; Compositions of derivatives of polycarbonates
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- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
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- C08K5/00—Use of organic ingredients
- C08K5/36—Sulfur-, selenium-, or tellurium-containing compounds
- C08K5/41—Compounds containing sulfur bound to oxygen
- C08K5/42—Sulfonic acids; Derivatives thereof
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K2201/017—Additives being an antistatic agent
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Abstract
The invention discloses a kind of preparation methods of silver nanowires modified fullerenes micro/nano-fibre, comprising: (1) prepares the fullerene micro/nano-fibre that draw ratio is about 1000；(2) it is acidified single step reaction of going forward side by side and obtains mercapto-functionalized fullerene micro nanometer fiber；(3) fullerene fiber that anchoring has platinum is prepared；(4) the silver nanowires modified fullerenes micro/nano-fibre of growth in situ silver nanowires is prepared.The present invention also provides a kind of silver nanowires modified fullerenes micro/nano-fibres, and its are used to prepare to obtain antistatic PC material.When reaching antistatic and requiring, antistatic agent dosage used in the present invention is few, problem of phase separation when overcoming fullerene micro/nano-fibre and silver nanowires blending and modifying between bring different component, and the probability that the present invention forms conductive network in matrix increases, the disadvantage big in intrinsic silicon contact resistance is overcome, the chemiluminescence of two kinds of antistatic agents is improved.
Description
Technical field
The present invention relates to a kind of fibrous materials and its preparation method and application, and in particular to a kind of modified fowler of silver nanowires
Alkene micro/nano-fibre, preparation method and applications belong to anti-static material technical field.
Background technique
Polycarbonate (PC) is a kind of unformed, odorless, nontoxic, the high grade of transparency nothing as one of five large-engineering plastics
Color is yellow thermoplastic, there is excellent impact resistance, and tensile strength, complete intensity, compressive strength are high, and there are also good
Heat resistance and lower temperature resistance keep stable mechanical property in wider temperature range.But PC ontology insulate, and surface is not inhaled
Water limits it in some applications for needing antistatic field.In recent years, many researchs are dedicated to the method with addition antistatic agent
Improve the antistatic property of PC material.
It include mainly carbon system and metal packing system as the antistatic agent of addition type, for added material nature,
It is best for the antistatic property for improving composite material using metal base antistatic agent, but metal added material is critical
Concentration is larger, generally 50% or so, it is therefore desirable to which amount is big, and cost increases；And Metal Substrate functional material add in large quantities with
And the two compatibility it is poor often to formed composite material mechanical performance and stability have an impact.Metal one-dimensional nano line
Conductive network more easily is formed in matrix polymer continuous phase under low concentration, to substantially reduce the use of metal packing
Amount weakens the adverse effect to basis material.In carbon system antistatic agent, fullerene micro/nano-fibre at present under study for action by
It attractes attention.Fullerene micro/nano-fibre electric conductivity is similar to graphite, and its draw ratio outstanding when that is added to it in matrix ratio is led
Electrical carbon is black to be more advantageous to the network structure that chain type is formed in matrix continuous phase, but its major defect be its in a polymer matrix
Dispersibility it is poor, need the organic modification on surface to improve surface polarity, improve dispersion in a polymer matrix and boundary
Face binding force.
In view of the advantage that both the above material is prominent, by growing silver nanoparticle in fullerene micro/nano-fibre surface in situ
Line obtains combining the composite antistatic agent of the two advantage, and is added in PC material, can effectively improve the antistatic of PC material
Property and reduce influence of the antistatic agent to polymeric matrix.
Summary of the invention
In order to overcome the above-mentioned deficiencies of the prior art, the present invention provides one kind based on silver nanowires modified fullerenes it is micro-/
Anti-static material of nanofiber and preparation method thereof.By growing silver nanowires in fullerene micro/nano-fibre surface in situ,
Composite anti-static material is prepared, and is distributed in PC matrix by dispersing agent, the antistatic property and drop of PC material are effectively improved
Influence of the low antistatic agent to polymeric matrix.
Cardinal principle of the invention is: by fullerene micro/nano-fibre surface sulfhydrylation, and utilizing the coordination of sulfydryl
Act on fullerene micro/nano-fibre surface anchoring platinum crystal seed, it is modified to prepare a kind of silver nanowires for growth in situ silver nanowires
Fullerene micro/nano-fibre antistatic agent, and be dispersed in PC matrix by dispersing agent, it is excellent to prepare antistatic property
PC material.
The present invention is specifically achieved in that
A kind of preparation method of silver nanowires modified fullerenes micro/nano-fibre, comprises the following steps that
(1) LLIP method is utilized, it is fine that the fullerene micro-/ nano that draw ratio is about 1000 is prepared in pyridine-Isopropanol Solvent
Dimension；
(2) acidification first is carried out to fullerene micro/nano-fibre, then with the fullerene micro-/ nano after acidification
Fiber and the polyfunctional group reactive organic molecule containing sulfydryl obtain mercapto-functionalized fullerene micro nanometer fiber；
(3) the fullerene micro/nano-fibre of sulfhydrylation is dispersed in ethylene glycol, the second of platinous chloride or chloroplatinic acid is added
Glycol solution, the mass ratio by hydrosulphonyl functionalized fullerene fiber and platinum element are 10000:(0.2~2) addition, 140~
10~30min is reacted under 180 DEG C of constant temperatures obtains the fullerene fiber that anchoring has platinum；
(4) after previous reaction, silver nitrate solution is added into solution and ethylene glycol containing structure directing agent is molten
Liquid, wherein the mass ratio of hydrosulphonyl functionalized fullerene micro nanometer fiber and silver element is in 1:(0.2~2), silver ion in solution
Molar ratio with structure directing agent is 1:(2~20), solution is warming up to 150~190 DEG C of 1~4h of isothermal reaction, is centrifugated,
Obtain the silver nanowires modified fullerenes micro/nano-fibre of growth in situ silver nanowires.
Further scheme is:
The specific steps of fullerene micro/nano-fibre preparation are as follows: fullerene is dissolved in pyridine solvent, 0~
10~60min of ultrasound in 35 DEG C of water baths, be made saturated solution, take it is a certain amount of above-mentioned saturated solution is mixed with isopropanol,
Mixed proportion is volume ratio 1:(1~25), it is put into 24~72h of complexing in -5 DEG C~20 DEG C of constant incubator, draw ratio is made
About 1000 fullerene micro/nano-fibre.
Further scheme is:
Step (2) specifically: by 1~3g prepare fullerene micro/nano-fibre is impregnated in the 50mL concentrated sulfuric acid be acidified 1~
3h is subsequently dispersed 2~4h of ultrasound in 150mL n,N-Dimethylformamide, and adding polyfunctional group of the 1~3g containing sulfydryl has
Machine molecule, and catalysis equivalent to 4- dimethylamino pyridine, filter and wash after 80~120 DEG C of 8~16h of reaction and be dried to obtain mercapto
The fullerene micro/nano-fibre of base functionalization.Wherein, the concentrated sulfuric acid refers to the sulfuric acid solution that mass fraction is greater than or equal to 70%.
The polyfunctional group organic molecule containing sulfydryl screened from thioacetic acid, to mercaptobenzoic acid and mercaptoethylmaine,
Selected structure directing agent is neopelex (SDBS), cetyl ammonium bromide (CTAB) and polyvinylpyrrolidone
(PVP) one such.
It the present invention also provides a kind of silver nanowires modified fullerenes micro/nano-fibre, is changed by above-mentioned silver nanowires
What the preparation method of property fullerene micro/nano-fibre was prepared.
The present invention also provides the application of silver nanowires modified fullerenes micro/nano-fibre, it is particularly used for being prepared
Antistatic PC material.
Further, concrete application is realized by the following method:
By PC, the fullerene micro/nano-fibre of silver nanowires functionalization, dispersing agent by weight 100:(0.1~1):
(0.1~0.3) mixes 5~15min in mixing machine with 10~40r/min, forms, obtains through double screw extruder melting extrusion
Antistatic PC material.
Selected dispersing agent is soluble polyurethane (WPU), neopelex (SDBS), polyvinylpyrrolidone
(PVP), cetyl trimethylammonium bromide (CTAB), any one in alkylphenol-polyethenoxy base ether or two kinds or more points
The combination of powder.
The mixing machine is GH-10 type mixing machine；The double screw extruder is SHJ-20 type double screw extruder.
Compared with prior art, used in the present invention anti-the beneficial effects of the present invention are: when reaching antistatic and requiring
Electrostatic agent dosage is few, when overcoming fullerene micro/nano-fibre and silver nanowires blending and modifying between bring different component
Problem of phase separation, and the present invention forms the probability increase of conductive network in matrix, overcomes in intrinsic silicon contact resistance
Big disadvantage improves the chemiluminescence of two kinds of antistatic agents.
Specific embodiment
The present invention is described in further detail combined with specific embodiments below.
Embodiment 1
A kind of preparation method of the fullerene micro/nano-fibre anti-static material modified based on silver nanowires includes:
Fullerene is dissolved in pyridine solvent, 10~60min of ultrasound in 0~35 DEG C of water bath, it is molten that saturation is made
Liquid takes a certain amount of above-mentioned saturated solution to mix with isopropanol, and mixed proportion is volume ratio 1:1~25, is put into constant incubator
Certain time, the fullerene micro/nano-fibre that obtained draw ratio is about 1000 is complexed.By the fiber of 1g preparation in the 50mL concentrated sulfuric acid
Middle immersion is acidified 2h, is subsequently dispersed ultrasound 2h in 150mL n,N-Dimethylformamide, adds 1g to mercaptobenzoic acid, and
Be catalyzed equivalent to 4- dimethylamino pyridine, filter and wash after 100 DEG C of reaction 12h and be dried to obtain mercapto-functionalized fullerene
Micro/nano-fibre.Again by 100g mercapto-functionalized fullerene micro/nano-fibre ultrasonic disperse into 100mL ethylene glycol, it is added
The platinum ion concentration of 10mL is the platinous chloride ethylene glycol solution of 1mg/mL, is warming up to 160 DEG C and isothermal reaction 10min, obtains
The fullerene micro/nano-fibre of platinum anchoring.After the reaction was completed, the poly- ethyl of 0.1mol/L silver nitrate solution and 0.5mol/L is added
Each 10mL of pyrrolidones ethylene glycol solution, then be warming up to 160 DEG C, isothermal reaction 2h, after centrifuge washing be dried to obtain Yin Na
The fullerene micro/nano-fibre of rice noodles growth in situ.By the modified fullerene micro/nano-fibre of PC, silver nanowires, dispersing agent ten
Dialkyl sulfonates are according to the ratio of mass ratio 1:0.1:0.1 with 15r/min mixing 15min, warp in GH-10 type mixing machine
SHJ-20 type double screw extruder melting extrusion molding, obtains antistatic PC material.The surface resistivity for measuring PC material is less than
500 Ω are good anti-static material；PC material transmissivity be greater than 90%, mist degree less than 1%, surface dynes value 36dye with
On, reach optical grade PC requirement.
Embodiment 2
A kind of preparation method of the fullerene micro/nano-fibre anti-static material modified based on silver nanowires includes:
Fullerene is dissolved in pyridine solvent, 10~60min of ultrasound in 0~35 DEG C of water bath, it is molten that saturation is made
Liquid takes a certain amount of above-mentioned saturated solution to mix with isopropanol, and mixed proportion is volume ratio 1:1~25, is put into constant incubator
Certain time, the fullerene micro/nano-fibre that obtained draw ratio is about 1000 is complexed.By the fiber of 1g preparation in the 50mL concentrated sulfuric acid
Middle immersion is acidified 2h, is subsequently dispersed ultrasound 2h in 150mL n,N-Dimethylformamide, adds 1.5g mercaptoethylmaine, and urge
Change equivalent to 4- dimethylamino pyridine, filter and wash after 100 DEG C of reaction 12h and be dried to obtain mercapto-functionalized fullerene
Micro/nano-fibre.Again by 100g mercapto-functionalized fullerene micro/nano-fibre ultrasonic disperse into 100mL ethylene glycol, it is added
The platinum ion concentration of 10mL is the platinous chloride ethylene glycol solution of 1mg/mL, is warming up to 160 DEG C and isothermal reaction 10min, obtains
The fullerene micro/nano-fibre of platinum anchoring.After the reaction was completed, the dodecane of 0.1mol/L silver nitrate solution and 0.5mol/L is added
Each 10mL of base benzene sulfonic acid sodium salt ethylene glycol solution, then be warming up to 160 DEG C, isothermal reaction 2h, after centrifuge washing be dried to obtain silver
The fullerene micro nanometer fiber of nano-thread in-situ growth.By PC, fullerene micro nanometer fiber, the dispersing agent of silver nanowires functionalization
Soluble polyurethane (WPU) is according to mass ratio 1:0.1:0.15: ratio mixed in GH-10 type mixing machine with 30r/min
5min is formed through SHJ-20 type double screw extruder melting extrusion, is measured the surface resistivity of PC material less than 500 Ω, is good
Good anti-static material；PC material transmissivity is greater than 90%, and for mist degree less than 1%, surface dynes value reaches light in 36dye or more
Classes and grades in school PC requirement.
It should be noted that various products and relevant parameter, various reaction partners and work used by embodiment as above
Skill condition is more typical example, but is verified by inventor's a large number of experiments, in the other differences of those listed above
The reaction partner of type and other process conditions etc. are also applicable, and attainable cost invents claimed technology effect
Fruit.
Although reference be made herein to invention has been described for explanatory embodiment of the invention, and above-described embodiment is only this hair
Bright preferable embodiment, embodiment of the present invention are not limited by the above embodiments, it should be appreciated that those skilled in the art
Member can be designed that a lot of other modification and implementations, these modifications and implementations will fall in principle disclosed in the present application
Within scope and spirit.
Claims (10)
1. a kind of preparation method of silver nanowires modified fullerenes micro/nano-fibre, it is characterised in that comprise the following steps that
(1) LLIP method is utilized, the fullerene micro/nano-fibre that draw ratio is about 1000 is prepared in pyridine-Isopropanol Solvent；
(2) acidification first is carried out to fullerene micro/nano-fibre, it is then further with the polyfunctional group organic molecule containing sulfydryl
Reaction obtains mercapto-functionalized fullerene micro/nano-fibre；
(3) mercapto-functionalized fullerene micro/nano-fibre is dispersed in ethylene glycol, the second of platinous chloride or chloroplatinic acid is added
The mass ratio of glycol solution, mercapto-functionalized fullerene micro/nano-fibre and platinum element is 10000:(0.2~2), 140
10~30min is reacted under~180 DEG C of constant temperatures obtains the mercapto-functionalized fullerene micro/nano-fibre that anchoring has platinum；
(4) after previous reaction, silver nitrate solution and the ethylene glycol solution containing structure directing agent are added into solution,
In mercapto-functionalized fullerene micro/nano-fibre and silver element mass ratio in 1:(0.2~2), silver ion and knot in solution
The molar ratio of structure directed agents is 1:(2~20), solution is warming up to 150~190 DEG C of 1~4h of isothermal reaction, is centrifugated, obtains
The silver nanowires modified fullerenes micro/nano-fibre of growth in situ silver nanowires.
2. the preparation method of silver nanowires modified fullerenes micro/nano-fibre according to claim 1, it is characterised in that:
Step (1) specifically: fullerene is dissolved in pyridine solvent, 10~60min of ultrasound in 0~35 DEG C of water bath,
Be made saturated solution, take it is a certain amount of above-mentioned saturated solution is mixed with isopropanol, mixed proportion be volume ratio 1:(1~25), put
Enter 24~72h of complexing, the fullerene micro/nano-fibre that obtained draw ratio is about 1000 in -5 DEG C~20 DEG C of constant incubator.
3. the preparation method of silver nanowires modified fullerenes micro/nano-fibre according to claim 1, it is characterised in that:
Step (2) specifically: 1~3g fullerene micro/nano-fibre prepared is impregnated into 1~3h of acidification in the 50mL concentrated sulfuric acid,
It is subsequently dispersed 2~4h of ultrasound in 150mL n,N-Dimethylformamide, adds organic point of polyfunctional group of the 1~3g containing sulfydryl
Son, and catalysis equivalent to 4- dimethylamino pyridine, filter and wash after 80~120 DEG C of 8~16h of reaction and be dried to obtain sulfydryl function
The fullerene micro/nano-fibre of energyization.
4. according to claim 1 or the preparation method of the 3 silver nanowires modified fullerenes micro/nano-fibres, it is characterised in that:
The polyfunctional group organic molecule containing sulfydryl screened from thioacetic acid, in mercaptobenzoic acid and mercaptoethylmaine appoint
It anticipates one kind.
5. the preparation method of silver nanowires modified fullerenes micro/nano-fibre according to claim 1, it is characterised in that:
Selected structure directing agent is neopelex, cetyl ammonium bromide and polyvinylpyrrolidone therein one
Kind.
6. a kind of silver nanowires modified fullerenes micro/nano-fibre, it is characterised in that be by any right of claim 1 to 5
It is required that the preparation method of the silver nanowires modified fullerenes micro/nano-fibre was prepared.
7. the application of silver nanowires modified fullerenes micro/nano-fibre described in claim 6, it is characterised in that: be used to prepare
To antistatic PC material.
8. the application of silver nanowires modified fullerenes micro/nano-fibre according to claim 7, it is characterised in that:
Using realizing by the following method:
By PC, the fullerene micro/nano-fibre of silver nanowires functionalization, dispersing agent by weight 100:(0.1~1): (0.1~
0.3) 5~15min is mixed with 10~40r/min in mixing machine, forms, obtains antistatic through double screw extruder melting extrusion
PC material.
9. the application of silver nanowires modified fullerenes micro/nano-fibre according to claim 8, it is characterised in that:
Selected dispersing agent is soluble polyurethane, neopelex, polyvinylpyrrolidone, cetyl trimethyl bromine
Change the combination of ammonium, any one in alkylphenol-polyethenoxy base ether or two kinds and the above dispersing agent.
10. the application of silver nanowires modified fullerenes micro/nano-fibre according to claim 8, it is characterised in that:
The mixing machine is GH-10 type mixing machine；The double screw extruder is SHJ-20 type double screw extruder.
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Cited By (1)
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| CN114275769A (en) * | 2021-12-15 | 2022-04-05 | 井冈山大学 | Method for separating C from fullerene mixture by utilizing silver salt60And C70Method (2) |
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| CN114275769A (en) * | 2021-12-15 | 2022-04-05 | 井冈山大学 | Method for separating C from fullerene mixture by utilizing silver salt60And C70Method (2) |
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Application publication date: 20190101 |