CN107385562A - A kind of alginic acid/Nano Silver composite nano fiber and preparation method thereof - Google Patents
A kind of alginic acid/Nano Silver composite nano fiber and preparation method thereof Download PDFInfo
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- CN107385562A CN107385562A CN201710568891.4A CN201710568891A CN107385562A CN 107385562 A CN107385562 A CN 107385562A CN 201710568891 A CN201710568891 A CN 201710568891A CN 107385562 A CN107385562 A CN 107385562A
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- nano
- silver
- alginic acid
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/04—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of alginates
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/0007—Electro-spinning
- D01D5/0015—Electro-spinning characterised by the initial state of the material
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/83—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with metals; with metal-generating compounds, e.g. metal carbonyls; Reduction of metal compounds on textiles
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M16/00—Biochemical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. enzymatic
- D06M16/006—Biochemical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. enzymatic with wool-protecting agents; with anti-moth agents
Abstract
The invention discloses a kind of alginic acid/Nano Silver composite nano fiber, described alginic acid/Nano Silver composite nano fiber is the sodium alginate nano fiber as made from method of electrostatic spinning, alginic acid silver nanoparticle fiber is made through ion exchange, restore made from silver ion, the inside and outer surface of described alginic acid/silver nano-grain composite nano fiber are evenly distributed with nano-Ag particles.The method for preparing the material successfully overcomes limitation of the spinnability to nano-Ag particles doping; avoid the problem of nano-Ag particles are reunited in electro-spinning process; this method can realize the large-scale production of the composite fibre containing Nano Silver; nano-Ag particles content is high in the composite nano fiber, and is uniformly distributed in material surface, and fibre diameter is small; specific surface area is big; superior performance, and be easily recycled, effectively save cost.
Description
Technical field
The invention belongs to technical field of nano material, and in particular to a kind of alginic acid/Nano Silver composite nano fiber and its
Preparation method.
Background technology
Functionalized nanoparticles are combined the composite prepared with electrostatic spinning because of the property such as its unique magnetic, light, electricity, catalysis
Extensive concern can be caused.In numerous work(performance nano particles, gold, silver, Pt nanoparticle have unique electricity, light
And catalytic performance.By taking nano-Ag particles as an example, Nano Silver causes a disease for tens of kinds to Escherichia coli, gonococcus, chlamydia trachomatis etc.
Microorganism has strong suppression and killing action, and will not produce drug resistance, the skin effect of nano silver particles, quantum chi
Very little effect etc., make it that also there are some special purposes, such as surface-enhanced Raman application, medical application.But simple receive
Rice Argent grain cost is higher and is not easily recycled recycling, limits the application prospect of material.
At present, can be using nano-Ag particles as antiseptic for the recovering effect for reducing cost, improving nano-Ag particles
It is doped to the composite nano fiber that loading nano silvery particle is prepared in electrospinning precursor liquid.But there is many weak points in this method.
In direct blending process, the doping of silver nano-grain is seriously restricted by spinnability；And nano particle is easily reunited, it is not easy to obtain
Uniform spinning precursor liquid is obtained, causes silver nano-grain skewness in the material, and the nanofiber diameter prepared is uneven
It is even, influence the performance of material.However, prepare sodium alginate nano fiber first using electrostatic spinning, in conjunction with ion exchange with
In-situ reducing self assembly, it can on a large scale prepare and carry silver-colored alginic acid nanofiber.Gained, which carries silver-colored alginic acid nanofiber, to be had
Fibre diameter is thin, and Argent grain content is high, is evenly distributed and does not reunite and the advantages that size tunable.
The content of the invention
The technical problem to be solved in the present invention is：Overcome prior art defect, there is provided a kind of alginic acid/Nano Silver is compound to be received
Rice fiber and preparation method thereof.This method successfully overcomes limitation of the spinnability to nano-Ag particles doping, avoids electrospinning
During nano-Ag particles reunite the problem of, this method can realize the large-scale production of the composite fibre containing Nano Silver, should
Nano-Ag particles content is high in composite nano fiber, and is uniformly distributed in material internal and surface, and fibre diameter is small, specific surface area
Greatly, superior performance, and be easily recycled, effectively save cost.
In order to solve the above problems, the invention provides a kind of alginic acid/Nano Silver composite nano fiber, described marine alga
Acid/Nano Silver composite nano fiber is the sodium alginate nano fiber as made from method of electrostatic spinning, and marine alga is made through ion exchange
Sour silver nanoparticle fiber, is restored made from silver ion, the inside of described alginic acid/silver nano-grain composite nano fiber and outer
Surface is evenly distributed with nano-Ag particles.
Preferably, the average diameter of described Na-alginate nanofiber is 170nm, and described alginic acid/Nano Silver is multiple
The average diameter for closing nanofiber is 207nm.
Preferably, described sodium alginate nano fiber is sodium alginate/PEO composite nano fiber.
The invention also discloses the preparation method of described sodium alginate/Nano Silver composite nano fiber, including following step
Suddenly：
(1) electrospinning sodium alginate nano fiber：The spinning precursor liquid containing sodium alginate is prepared, is prepared with method of electrostatic spinning
Sodium alginate nano fiber film；
(2) load silver ion：Sodium alginate nano fiber made from step (1) is dipped in silver nitrate solution, makes fiber
Internal and surface sodium ion and silver ion progress ion exchange, obtain alginic acid silver nanoparticle fiber, sample are taken out, spend from
Sub- water cleaning sample；
(3) silver ion is reduced：Sample obtained by step (2) is dipped in reductant solution reduce fibrous inside and it is internal and
The silver ion on surface, inside the sodium alginate nano fiber and after surface forms silver nano-grain, with deionized water cleaning sample,
Drying sample produces alginic acid/Nano Silver composite nano fiber.
The fiber of the present invention prepares sodium alginate nano fiber first in preparation process using electrostatic spinning, in conjunction with
Ion exchange and in-situ reducing self assembly, this method successfully overcome limitation of the spinnability to nano-Ag particles doping, avoided
The problem of nano-Ag particles are reunited in electro-spinning process, this method can realize the scale metaplasia of the composite fibre containing Nano Silver
Production, meanwhile, sodium alginate nano fiber diameter small specific surface product can fully contact greatly carry out ion exchange with silver nitrate solution,
The abundant load silver ion in inside and surface of fiber, the silver ion loaded are reduced further into silver nano-grain so that gained
The silver nano-grain content height of silver-colored alginic acid nanofiber is carried, nano-Ag particles are uniform in the inside of fiber and surface distributed, and
Composite fibre directly remains as nanoscale, it may have and larger specific surface area causes there is more contact sites between fiber,
Make material that there is superior electric property.Furthermore, it is possible to by set-up procedure (2) load silver ion and step (3) reduce silver from
Son test parameters adjustment control composite nano fiber nano-Ag particles particle diameter, so as to be adjusted flexibly the performance of material and
Pattern.
Preferably, lead in the spinning precursor liquid in described step (1) containing Qula, described sodium alginate nano fiber
For sodium alginate and the compound composite nano fiber of other high molecular weight water soluble polymers.
Method of electrostatic spinning prepares pure sodium alginate fiber and certain difficulty be present, and adding water soluble polymer can strengthen
The spinnability of sodium alginate, it is easier to obtained sodium alginate composite fiber, and the water solubility in sodium alginate composite fiber is high
Molecular material can be dissolved in reaction solution during follow-up being dipped in reaction solution carries out ion exchange load silver ion, will not
Influence the alginic acid/constituent of Nano Silver composite nano fiber and the structural behaviour of fiber of final gained.
Preferably, described step (1) electrospinning sodium alginate nano fiber：At normal temperatures, sodium alginate powder 0.5 is weighed
~2g, add in container, add 0.1~0.2g PEOs (PEO), 0.4~0.5g Qulas are led to, and 2~3g dimethyl is sub-
Sulfone, 30~40g deionized waters, stir at normal temperatures to solution homogeneous transparent and obtain spinning precursor liquid, spinning precursor liquid is injected quiet
In electric spinning device, sodium alginate nano fiber is prepared with method of electrostatic spinning, 10~15kV of spinning voltage, spinning distance 12~
18cm, 20~30min of spinning time, sodium alginate nano fiber obtained by electrospinning are placed in baking oven to be placed in 40~60 DEG C of baking ovens and done
Dry 1~3h.
Preferably, described step (2) load silver ion：Silver nitrate aqueous solution is configured, in described silver nitrate aqueous solution
The content of silver nitrate is 20~30wt%, and sodium alginate nano fiber made from step (1) is dipped in silver nitrate aqueous solution, leaching
Bubble 20~30 minutes, uses deionized water rinsing 2~3 times after taking-up.
Preferably, described step (3) reduction silver ion：Sample obtained by step (2) is dipped in dimethylamino borine water
The silver ion of fiber surface is reduced in solution, the content of methylamino borine is 5 × 10 in the described methylamino borine aqueous solution- 2Wt%, soak 10~20 minutes, be placed in for 3~4 times with deionized water rinsing drying 2~5h in 50 DEG C of baking ovens after taking-up, produced
Alginic acid/Nano Silver composite nano fiber.
The beneficial effects of the invention are as follows：The invention provides a kind of alginic acid/Nano Silver composite nano fiber and its preparation
Method.This method successfully overcomes limitation of the spinnability to nano-Ag particles doping, avoids Nano Silver in electro-spinning process
The problem of grain is reunited, this method can realize the large-scale production of the composite fibre containing Nano Silver, in the composite nano fiber
Nano-Ag particles content is high, and is uniformly distributed in material internal and surface, and fibre diameter is small, and specific surface area is big, superior performance, and
It is easily recycled, effectively save cost.
(1) fiber of the invention prepares sodium alginate nano fiber, then tie first in preparation process using electrostatic spinning
Ion exchange and in-situ reducing self assembly are closed, this method successfully overcomes limitation of the spinnability to nano-Ag particles doping, kept away
The problem of nano-Ag particles are reunited in electro-spinning process is exempted from, this method can realize the scale of the composite fibre containing Nano Silver
Production, meanwhile, sodium alginate nano fiber diameter small specific surface product can fully contact greatly carry out ion exchange with silver nitrate solution,
In the abundant load silver ion in the inside of fiber and surface, the silver ion loaded is reduced further into silver nano-grain so that institute
The silver nano-grain content height of silver-colored alginic acid nanofiber must be carried, nano-Ag particles are uniform in the inside of fiber and surface distributed,
And the direct of composite fibre remains as nanoscale, it may have larger specific surface area causes there is more contact positions between fiber
Point, make material that there is superior electric property.
(2) the adjustment control of the test parameters of silver ion can be reduced by set-up procedure (2) load silver ion and step (3)
The particle diameter of the nano-Ag particles of composite nano fiber processed, so as to which the performance of material and pattern be adjusted flexibly.
(3) method of electrostatic spinning prepares pure sodium alginate fiber and certain difficulty be present, and adding water soluble polymer can be with
Strengthen the spinnability of sodium alginate, it is easier to obtained sodium alginate composite fiber, and it is water-soluble in sodium alginate composite fiber
Property high polymer material it is follow-up be dipped in reaction solution carry out ion exchange load silver ion during can be dissolved in reaction solution,
Alginic acid/the constituent of Nano Silver composite nano fiber and the structural behaviour of fiber of final gained are not interfered with.
(4) method that this method prepares silver-carrying nano fiber compared to other electrospinnings, preparation method is simpler, cost compared with
It is low, and gained fiber nano silver material content is higher, superior performance, meanwhile, nano-Ag particles, which are bound, to be limited on fiber, more
Add convenient recovery and utilize, there is good application prospect.
Brief description of the drawings
Fig. 1：The electron scanning micrograph of sodium alginate nano fiber；
Fig. 2：The diameter distribution statisticses figure of sodium alginate nano fiber；
Fig. 3：The electron scanning micrograph of alginic acid/Nano Silver composite nano fiber；
Fig. 4：The diameter distribution statisticses figure of alginic acid/Nano Silver composite nano fiber；
Fig. 5：The XRD of sodium alginate nano fiber and alginic acid/Nano Silver composite nano fiber.
Embodiment
For the technical characterstic for illustrating this programme can be understood, this programme is illustrated below by embodiment.
Embodiment 1
A kind of preparation method of sodium alginate/Nano Silver composite nano fiber, comprises the following steps：
(1) electrospinning sodium alginate nano fiber：At normal temperatures, sodium alginate powder 0.64g is weighed, is added in container, then
0.16g PEOs (PEO) are added, 0.4g Qulas are led to, and 2g dimethyl sulfoxide (DMSO)s, 36.8g deionized waters, stir 3h at normal temperatures
Spinning precursor liquid is obtained, spinning precursor liquid is injected in electrostatic spinning apparatus, sodium alginate nano fiber is prepared with method of electrostatic spinning,
Spinning voltage 12kV, spinning distance 15cm, spinning time 25min, sodium alginate nano fiber obtained by electrospinning, which is placed in baking oven, to be put
2h is dried in 50 DEG C of baking ovens, gained tunica fibrosa is cut to 2 × 2cm2Small pieces it is standby, the sodium alginate obtained by step (1)
The shape characteristic of nanofiber is as shown in figure 1, the average diameter of the fiber is 170nm (as shown in Figure 2)；
(2) load silver ion：Silver nitrate aqueous solution is configured, the content of silver nitrate is in described silver nitrate aqueous solution
30wt%, sodium alginate nano fiber made from step (1) is dipped in silver nitrate aqueous solution, soaks 20 minutes, used after taking-up
Deionized water rinsing 3 times；
(3) silver ion is reduced：Sample obtained by step (2) is dipped in the dimethylamino borine aqueous solution and reduces fibrous inside
With the silver ion on surface, the content of methylamino borine is 5 × 10 in the described methylamino borine aqueous solution-2Wt%, soak 15 points
Clock, it is placed in for 3 times with deionized water rinsing drying 3h in 50 DEG C of baking ovens after taking-up, produces sodium alginate/Nano Silver composite Nano
Fiber, the shape characteristic of gained alginic acid/Nano Silver composite nano fiber is as shown in figure 3, the average diameter of the fiber is 207nm
(as shown in Figure 2).
Alginic acid/Nano Silver described in the sodium alginate as made from above method/Nano Silver composite nano fiber is compound to be received
Rice fiber is the sodium alginate nano fiber as made from method of electrostatic spinning, and alginic acid silver nanoparticle fiber is made through ion exchange, then
Reduce made from silver ion, the inside and outer surface of described alginic acid/silver nano-grain composite nano fiber are uniformly distributed
There are nano-Ag particles.The sodium alginate nano fiber of gained and XRD such as Fig. 5 institutes of alginic acid/Nano Silver composite nano fiber
Show, the area load of the material nano-Ag particles it can be seen from Fig. 5 characteristic peak.
Illustrative embodiments are only not the restrictions to technical scheme described in the invention for understanding that the present invention is used,
Those of ordinary skill about field, on the basis of technical scheme described in claim, a variety of changes or change can also be made
Shape, all equivalent changes or deformation should all be covered within the claims of the present invention.It is not described in detail by the present invention
Place, it is the known technology of those skilled in the art of the present technique.
Claims (8)
1. a kind of alginic acid/Nano Silver composite nano fiber, it is characterised in that described alginic acid/Nano Silver composite Nano is fine
Dimension is the sodium alginate nano fiber as made from method of electrostatic spinning, and alginic acid silver nanoparticle fiber is made through ion exchange, restores
Made from silver ion, the inside and outer surface of described alginic acid/silver nano-grain composite nano fiber are all evenly distributed with and received
Rice Argent grain.
A kind of 2. alginic acid/Nano Silver composite nano fiber as claimed in claim 1, it is characterised in that described alginic acid
The average diameter of nanofiber received is 170nm, and the average diameter of described alginic acid/Nano Silver composite nano fiber is 207nm.
3. such as a kind of alginic acid/Nano Silver composite nano fiber as claimed in claim 1, it is characterised in that described marine alga
Sour sodium nanofiber is sodium alginate/PEO composite nano fiber.
4. a kind of preparation method of alginic acid/Nano Silver composite nano fiber as claimed any one in claims 1 to 3, its
It is characterised by, comprises the following steps：
(1) electrospinning sodium alginate nano fiber：The spinning precursor liquid containing sodium alginate is prepared, marine alga is prepared with method of electrostatic spinning
Sour sodium nano fibrous membrane；
(2) load silver ion：Sodium alginate nano fiber made from step (1) is dipped in silver nitrate solution, makes fibrous inside
Ion exchange is carried out with silver ion with the sodium ion on surface, alginic acid silver nanoparticle fiber is obtained, sample is taken out, uses deionized water
Cleaning sample；
(3) silver ion is reduced：Sample obtained by step (2) is dipped in reduced in reductant solution the silver on fibrous inside and surface from
Son, inside sodium alginate nano fiber and after surface formation silver nano-grain, with deionized water cleaning sample, drying sample is
Obtain alginic acid/Nano Silver composite nano fiber.
A kind of 5. preparation method of alginic acid/Nano Silver composite nano fiber as claimed in claim 4, it is characterised in that institute
Lead in spinning precursor liquid in the step of stating (1) containing Qula, described sodium alginate nano fiber be sodium alginate with it is other
The compound composite nano fiber of high molecular weight water soluble polymer.
A kind of 6. preparation method of alginic acid/Nano Silver composite nano fiber as claimed in claim 5, it is characterised in that institute
The step of stating (1) electrospinning sodium alginate nano fiber：At normal temperatures, 0.5~2g of sodium alginate powder is weighed, is added in container,
0.1~0.2g PEO are added, 0.4~0.5g Qulas are led to, 2~3g dimethyl sulfoxide (DMSO)s, 30~40g deionized waters, at normal temperatures
Stirring to solution homogeneous transparent obtains spinning precursor liquid, spinning precursor liquid is injected in electrostatic spinning apparatus, with electrostatic spinning legal system
Standby sodium alginate nano fiber, 10~15kV of spinning voltage, spinning 12~18cm of distance, 20~30min of spinning time, electrospinning institute
Sodium alginate nano fiber be placed in baking oven be placed in 40~60 DEG C of baking ovens dry 1~3h.
A kind of 7. preparation method of alginic acid/Nano Silver composite nano fiber as claimed in claim 4, it is characterised in that institute
The step of stating (2) load silver ion：Configure silver nitrate aqueous solution, in described silver nitrate aqueous solution the content of silver nitrate for 20~
30wt%, sodium alginate nano fiber made from step (1) is dipped in silver nitrate aqueous solution, soaked 20~30 minutes, taken out
Deionized water rinsing is used afterwards 2~3 times.
A kind of 8. preparation method of alginic acid/Nano Silver composite nano fiber as claimed in claim 4, it is characterised in that institute
The step of stating (3) reduces silver ion：Sample obtained by step (2) is dipped in the dimethylamino borine aqueous solution and reduces fibrous inside
With the silver ion on surface, the content of methylamino borine is 5 × 10 in the described methylamino borine aqueous solution-2Wt%, immersion 10~
20 minutes, it is placed in for 3~4 times with deionized water rinsing drying 2~5h in 50 DEG C of baking ovens after taking-up, produces alginic acid/Nano Silver
Composite nano fiber.
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Cited By (6)
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| CN107875432A (en) * | 2018-01-17 | 2018-04-06 | 嘉兴学院 | A kind of composite nano fiber antiseptic dressing and preparation method thereof |
| CN108193321A (en) * | 2017-12-13 | 2018-06-22 | 青岛海赛尔新材料科技有限公司 | Antibiotic property silver sulfate alginate fibre and preparation method thereof |
| CN109235027A (en) * | 2018-10-17 | 2019-01-18 | 江苏阳光股份有限公司 | A kind of nano silver method for sorting of antibacterial wool fabric |
| CN109402839A (en) * | 2018-11-18 | 2019-03-01 | 南通源佑纺织科技有限公司 | A kind of antibacterial polyester fibre lining cloth and its production technology |
| CN110567359A (en) * | 2019-08-01 | 2019-12-13 | 广东工业大学 | multi-stimulation self-sensing software driver based on shape memory and preparation method and application thereof |
| CN111321484A (en) * | 2018-12-14 | 2020-06-23 | 中国科学院大连化学物理研究所 | Strong ionic conductivity porous composite nanofiber and preparation method and application thereof |
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