CN106498559B - A kind of method that nanofiber is self-assembled into using small-molecular-weight sodium alginate - Google Patents
A kind of method that nanofiber is self-assembled into using small-molecular-weight sodium alginate Download PDFInfo
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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
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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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Abstract
The invention discloses a kind of methods that nanofiber is self-assembled into using small-molecular-weight sodium alginate, include the following steps：The sodium alginate of macromolecule is first degraded into the sodium alginate of small-molecular-weight；The sodium alginate of small-molecular-weight is added into deionized water dissolving afterwards；Finally, sodium alginate soln is stood, by self assembly, obtains being stored in the sodium alginate nano fiber in solution system.That is, by the sodium alginate molecule chain aggregation of degrade solubilising, small-molecular-weight, so as to which self assembly occur, after multistage self assembly, obtain it is finely dispersed, can be used for preparing high intensity, good thixotropic hydrogel sodium alginate nano fiber.The present invention is by simply regulating and controlling the molecular weight of sodium alginate, without adding any crosslinking agent or electrolyte salt, you can be self-assembled into nanofiber.Preparation method is simple, direct, efficient.Particularly, prepared sodium alginate nano fiber is " pure " sodium alginate ingredient.
Description
Technical field
Preparation method more particularly to a kind of use small-molecular-weight seaweed the present invention relates to a kind of sodium alginate nano fiber
The method that sour sodium is self-assembled into nanofiber.
Background technology
Sodium alginate (Sodium Alginate, SA) also known as sodium alginate, it be by beta-D-mannuronic acid (M sections) and
The Natural linear macromolecule that α-L- guluronic acids (G sections) are formed by 1-4 glucosides key connections.
Since sodium alginate has good biocompatibility, degradability, strong hygroscopicity and hemostatic so that it is in medicine
It has a wide range of applications in object release, organizational project.Wherein, using sodium alginate as raw material, manufactured nanofiber, due to
It makes it have higher utility value in fields such as organizational project, drug releases with very high mass-surface ratio.
In the prior art, the preparation of sodium alginate nano fiber can only be made by electrospinning process.
Since sodium alginate strand is in rigidity, stretches in the solution, lack necessary chain entanglement effect, in its Static Spinning
In the preparation of silk liquid, generally require to add crosslinking agent or a large amount of water-soluble flexible macromolecules into sodium alginate soln system,
The viscosity of sodium alginate spinning solution can be made to reach the technological requirement of electrostatic spinning shapes, so ensure electrostatic spinning it is smooth into
Row.
It is not difficult to find out, the main problem of electrostatic spinning or is disadvantageous in that：When the preparation process of spinning solution it is complicated and
The control difficulty of technological parameter is big, correspondingly, often result in product quality (performance indicator, fiber morphology etc.) stability difference or
Fluctuation is big；Second is that electrospinning device cost is high, operating cost is relatively higher；Third, the diameter ratio of obtained nanofiber
It is larger, generally all on hundreds of nanometers.It is said on stricti jurise, " nanometer " fiber can not be referred to as.
Invention content
Short, simple for process easily-controllable, energy conservation and environmental protection, required instrument/set it is an object of the present invention to provide a kind of technological process
It is standby simple, manufacturing cost is cheap, good product quality, and is received convenient for preserving to be self-assembled into using small-molecular-weight sodium alginate for a long time
The method of rice fiber.
Present invention technical solution used for the above purpose is, a kind of to use small-molecular-weight sodium alginate self assembly
Into the method for nanofiber, which is characterized in that include the following steps：
The first step, the preparation of the sodium alginate of small-molecular-weight：
In proportion, the sodium alginate of macromolecule is added in deionized water, agitated swelling, dissolving obtain quality
Percent concentration is 1.5% sodium alginate soln A；
Then, hydrogen peroxide is added in, obtains mixed solution, the mass fraction of hydrogen peroxide is 1.5%~2% in mixed solution；
By mixed solution heating water bath to 65 DEG C, it is stirred to react 1h~15h；
Again in the ratio that the volume ratio of mixed solution and absolute ethyl alcohol is 1 ︰ 2, absolute ethyl alcohol is added in into mixed solution, is sunk
It forms sediment, centrifugation, obtains with small-molecular-weight sodium alginate solid content as main component；
Gained solid content is added into deionized water dissolving, then successively after dialysing, being freeze-dried, obtains purer small point
The sodium alginate powder of son amount；
Second step, sodium alginate nano fiber self assembly step：
The sodium alginate powder of gained small-molecular-weight is added into deionized water dissolving while stirring, obtains mass percent concentration
For 5%~60% sodium alginate soln B；
Third walks, and gained sodium alginate soln B is stood 2h~120h, is self-assembled into sodium alginate nano fiber；
The sodium alginate of above-mentioned macromolecule refers to sodium alginate of the weight average molecular weight in 313kDa~586kDa；
The sodium alginate of above-mentioned small-molecular-weight refers to the sodium alginate that weight average molecular weight is 23kDa~96kDa.
The technical effect brought directely by the technical proposal is that dexterously by simply regulating and controlling the molecular weight of sodium alginate,
Any crosslinking agent or electrolyte salt need not be added, nanofiber is self-assembled into using small-molecular-weight sodium alginate.Its preparation side
Method is simple, direct, efficient.Particularly, prepared sodium alginate nano fiber is " pure " sodium alginate ingredient, from cover to cover
Ground remains sodium alginate such as：The good characteristics such as degradability, compatibility.
It is not difficult to find out, the preparation method of above-mentioned technical proposal, technological process is short, simple for process easily-controllable, energy conservation and environmental protection, institute
It needs that instruments/equipment is simple, manufacturing cost is cheap, good product quality, and is preserved convenient for long-term.
To more fully understand the technical characterstic of the present invention, it is explained in detail and illustrates from principle below.
Sodium alginate is soluble easily in water.But due to the restriction of the high molecular high viscous characteristic factor of sodium alginate so that its is molten
Xie Du is relatively low.When it is in water solution system, when (sodium alginate) concentration reaches a certain level, it will gelation occurs.This
It is exactly the sodium alginate limited basic reason of solubility in water.
Based on the understanding to above-mentioned objective law, we have found under study for action, when sodium alginate passes through degradation, molecular weight
When a certain range is greatly reduced to, not only the solubility of sodium alginate in water can dramatically increase；Moreover, sodium alginate molecule
After chain shortens, rigidity substantially enhances；When the concentration of this sodium alginate in aqueous solution reaches certain critical value, alginic acid
Orientation aggregation will occur for sodium molecule chain, so as to which self assembly occur, form new structure, i.e. nanofiber.
It is important to note that the sodium alginate nano fiber obtained by the preparation method of above-mentioned technical proposal can be grown
Temporally, it steadily uniformly disperse/is stored in solution system (without additional " separation " step), thus convenient for storage.It is former
Because being：
Sodium alginate is one by unordered in aqueous solution by the transition process of random coil structure to nanofibrous structures
To orderly process, this is the process that an entropy subtracts.
In this course, because the reduction of the molecular weight of sodium alginate causes solubility to greatly increase, a large amount of seaweed
Sour sodium flocks together, therefore the hydrophobic effect of sodium alginate increases, and hydrophobic effect provides energy so that part sodium alginate
Strand being combined together tightly with sodium alginate strand, forms new structure, i.e. nanofibrous structures；
And nanofibrous structures are a kind of structures of stabilization, it is assumed that this nanofibrous structures to be made to change back to again original
Random coil structure then needs to provide energy, with the combination of hydrophobic effect.
Then it is still that an entropy subtracts process, it is also desirable to extraneous assuming that this nanofiber to be made to reassociate (length is thick, becomes larger)
Energy is provided.
Therefore, the sodium alginate nano fiber being present in solution system obtained by above-mentioned technical proposal, structure are
Stable, its destructive process is non-spontaneous.
That is, the preparation method of above-mentioned technical proposal, obtained sodium alginate nano fiber can for a long time,
Steadily uniformly disperse/be stored in solution system, be have theoretical foundation, be reliable.
Preferably, the above-mentioned method that nanofiber is self-assembled into using small-molecular-weight sodium alginate, which is characterized in that institute
A diameter of 50nm~the 800nm of sodium alginate nano fiber obtained, length are 3000nm~20000nm.
What the optimal technical scheme was directly brought has the technical effect that, a diameter of 50nm~800nm of sodium alginate nano fiber,
Length is 3000nm~20000nm, suitable for preparing high intensity, good thixotropic hydrogel, has very wide market
Application prospect.
Based on above-mentioned analysis, it can be appreciated that the key problem in technology point of the present invention includes：The rationally molecule of control sodium alginate
Amount, concentration and built-up time.
In conclusion the present invention relative to the prior art, has, technological process is short, simple for process, easily-controllable, energy conservation and environmental protection,
Required instruments/equipment is simple, and manufacturing cost is cheap, good product quality, and convenient for advantageous effects such as long-term preservations.
Description of the drawings
Fig. 1 is the self assembly principle schematic of the present invention；
Fig. 2 is the transmission electron microscope photo of the sodium alginate nano fiber obtained by embodiment 2.
Specific embodiment
With reference to embodiment, the present invention is described in detail.
Explanation：
1st, in following embodiment, sodium alginate raw material (that is, described " sodium alginate of macromolecule ") used is
Commercial product；H2O2It is commercial product with absolute ethyl alcohol.
2nd, in following embodiment, " sodium alginate of macromolecule " and " sodium alginate of small-molecular-weight ", point
Son amount is all measured using gel permeation chromatography (GPC).
3rd, in following embodiment, the pattern of sodium alginate nano fiber is the observed result under petrographic microscope；It is fine
Dimension diameter and fibre length are the observed result under transmission electron microscope.
Embodiment 1
Preparation method includes three steps as shown in Figure 1：
The first step, the preparation of the sodium alginate of small-molecular-weight：
In proportion, the sodium alginate (weight average molecular weight 313kDa) of macromolecule is added in deionized water, through stirring
Swelling, dissolving are mixed, obtains the sodium alginate soln A that mass percent concentration is 1.5%；
Then, hydrogen peroxide is added in, obtains mixed solution, the mass fraction of hydrogen peroxide is 1.5% in mixed solution；
By mixed solution heating water bath to 65 DEG C, it is stirred to react 12h；
Again in the ratio that the volume ratio of mixed solution and absolute ethyl alcohol is 1 ︰ 2, absolute ethyl alcohol is added in into mixed solution, is sunk
It forms sediment, centrifugation, obtains with small-molecular-weight sodium alginate solid content as main component；
Gained solid content is added into deionized water dissolving, then successively after dialysing, being freeze-dried, obtains purer small point
The sodium alginate powder (weight average molecular weight 74kDa) of son amount；
Second step, sodium alginate nano fiber self assembly step：
The sodium alginate powder of gained small-molecular-weight is added into deionized water dissolving while stirring, obtains mass percent concentration
For 10% sodium alginate soln B；
Third walks, and gained sodium alginate soln B is stood 72h, is self-assembled into sodium alginate nano fiber.
Products obtained therefrom is respectively placed under petrographic microscope and transmission electron microscope and is observed, the results show that sodium alginate Nanowire
It is line style or branching type to tie up pattern；Nanofiber diameter is 140~150nm, and length is 3500~3700nm.
Embodiment 2
Preparation method includes three steps as shown in Figure 1：
The first step, the preparation of the sodium alginate of small-molecular-weight：
In proportion, the sodium alginate (weight average molecular weight 586kDa) of macromolecule is added in deionized water, through stirring
Swelling, dissolving are mixed, obtains the sodium alginate soln A that mass percent concentration is 1.5%；
Then, hydrogen peroxide is added in, obtains mixed solution, the mass fraction of hydrogen peroxide is 1.5% in mixed solution；
By mixed solution heating water bath to 65 DEG C, it is stirred to react 15h；
Again in the ratio that the volume ratio of mixed solution and absolute ethyl alcohol is 1 ︰ 2, absolute ethyl alcohol is added in into mixed solution, is sunk
It forms sediment, centrifugation, obtains with small-molecular-weight sodium alginate solid content as main component；
Gained solid content is added into deionized water dissolving, then successively after dialysing, being freeze-dried, obtains purer small point
The sodium alginate powder (weight average molecular weight 95kDa) of son amount；
Second step, sodium alginate nano fiber self assembly step：
The sodium alginate powder of gained small-molecular-weight is added into deionized water dissolving while stirring, obtains mass percent concentration
For 10% sodium alginate soln B；
Third walks, and gained sodium alginate soln B is stood 120h, is self-assembled into sodium alginate nano fiber.
Products obtained therefrom is placed under petrographic microscope and is observed, the results show that sodium alginate nano fiber pattern for line style or
Branching type；
Products obtained therefrom is placed in observation under transmission electron microscope to can be seen that：Nanofiber diameter is 50~65nm, and length is
3200~3500nm.
Fig. 2 is the transmission electron microscope picture of obtained sodium alginate nano fiber.Apparent fiber knot as can see from Figure 2
Structure, this illustrates that products therefrom is nanofiber.
Embodiment 3
Preparation method includes three steps as shown in Figure 1：
The first step, the preparation of the sodium alginate of small-molecular-weight：
In proportion, the sodium alginate (weight average molecular weight 425kDa) of macromolecule is added in deionized water, through stirring
Swelling, dissolving are mixed, obtains the sodium alginate soln A that mass percent concentration is 1.5%；
Then, hydrogen peroxide is added in, obtains mixed solution, the mass fraction of hydrogen peroxide is 1.5% in mixed solution；
By mixed solution heating water bath to 65 DEG C, it is stirred to react 5h；
Again in the ratio that the volume ratio of mixed solution and absolute ethyl alcohol is 1 ︰ 2, absolute ethyl alcohol is added in into mixed solution, is sunk
It forms sediment, centrifugation, obtains with small-molecular-weight sodium alginate solid content as main component；
Gained solid content is added into deionized water dissolving, then successively after dialysing, being freeze-dried, obtains purer small point
The sodium alginate powder (weight average molecular weight 86kDa) of son amount；
Second step, sodium alginate nano fiber self assembly step：
The sodium alginate powder of gained small-molecular-weight is added into deionized water dissolving while stirring, obtains mass percent concentration
For 10% sodium alginate soln B；
Third walks, and gained sodium alginate soln B is stood 96h, is self-assembled into sodium alginate nano fiber.
Products obtained therefrom is respectively placed under petrographic microscope and transmission electron microscope and is observed, it can be seen that：Sodium alginate Nanowire
It is line style or branching type to tie up pattern；Nanofiber diameter is 55~70nm, and length is 4200~4500nm.
Embodiment 4
Preparation method includes three steps as shown in Figure 1：
The first step, the preparation of the sodium alginate of small-molecular-weight：
In proportion, the sodium alginate (weight average molecular weight 505kDa) of macromolecule is added in deionized water, through stirring
Swelling, dissolving are mixed, obtains the sodium alginate soln A that mass percent concentration is 1.5%；
Then, hydrogen peroxide is added in, obtains mixed solution, the mass fraction of hydrogen peroxide is 1.5% in mixed solution；
By mixed solution heating water bath to 65 DEG C, it is stirred to react 8h；
Again in the ratio that the volume ratio of mixed solution and absolute ethyl alcohol is 1 ︰ 2, absolute ethyl alcohol is added in into mixed solution, is sunk
It forms sediment, centrifugation, obtains with small-molecular-weight sodium alginate solid content as main component；
Gained solid content is added into deionized water dissolving, then successively after dialysing, being freeze-dried, obtains purer small point
The sodium alginate powder (weight average molecular weight 91kDa) of son amount；
Second step, sodium alginate nano fiber self assembly step：
The sodium alginate powder of gained small-molecular-weight is added into deionized water dissolving while stirring, obtains mass percent concentration
For 10% sodium alginate soln B；
Third walks, and gained sodium alginate soln B is stood 72h, is self-assembled into sodium alginate nano fiber.
Products obtained therefrom is respectively placed under petrographic microscope and transmission electron microscope and is observed, it can be seen that：Sodium alginate Nanowire
It is line style or branching type to tie up pattern；Nanofiber diameter is 165~180nm, and length is 4000~4500nm.
Embodiment 5
Preparation method includes three steps as shown in Figure 1：
The first step, the preparation of the sodium alginate of small-molecular-weight：
In proportion, the sodium alginate (weight average molecular weight 313kDa) of macromolecule is added in deionized water, through stirring
Swelling, dissolving are mixed, obtains the sodium alginate soln A that mass percent concentration is 2%；
Then, hydrogen peroxide is added in, obtains mixed solution, the mass fraction of hydrogen peroxide is 1.5% in mixed solution；
By mixed solution heating water bath to 65 DEG C, it is stirred to react 4h；
Again in the ratio that the volume ratio of mixed solution and absolute ethyl alcohol is 1 ︰ 2, absolute ethyl alcohol is added in into mixed solution, is sunk
It forms sediment, centrifugation, obtains with small-molecular-weight sodium alginate solid content as main component；
Gained solid content is added into deionized water dissolving, then successively after dialysing, being freeze-dried, obtains purer small point
The sodium alginate powder (weight average molecular weight 23kDa) of son amount；
Second step, sodium alginate nano fiber self assembly step：
The sodium alginate powder of gained small-molecular-weight is added into deionized water dissolving while stirring, obtains mass percent concentration
For 10% sodium alginate soln B；
Third walks, and gained sodium alginate soln B is stood 72h, is self-assembled into sodium alginate nano fiber.
Products obtained therefrom is respectively placed under petrographic microscope and transmission electron microscope and is observed, it can also be seen that：Sodium alginate is received
Rice fiber morphology is line style or branching type；Nanofiber diameter is 50~200nm, and length is 3000~5500nm.
Claims (2)
- A kind of 1. method that nanofiber is self-assembled into using small-molecular-weight sodium alginate, which is characterized in that include the following steps：The first step, the preparation of the sodium alginate of small-molecular-weight：In proportion, the sodium alginate of macromolecule is added in deionized water, agitated swelling, dissolving obtain quality percentage Specific concentration is 1.5% sodium alginate soln A；Then, hydrogen peroxide is added in, obtains mixed solution, the mass fraction of hydrogen peroxide is 1.5%~2% in mixed solution；By mixed solution heating water bath to 65 DEG C, it is stirred to react 1h~15h；Again in the ratio that the volume ratio of mixed solution and absolute ethyl alcohol is 1 ︰ 2, absolute ethyl alcohol is added in into mixed solution, precipitate, Centrifugation, obtains with small-molecular-weight sodium alginate solid content as main component；Gained solid content is added into deionized water dissolving, then successively after dialysing, being freeze-dried, obtains purer small-molecular-weight Sodium alginate powder；Second step, sodium alginate nano fiber self assembly step：The sodium alginate powder of gained small-molecular-weight is added into deionized water dissolving while stirring, obtaining mass percent concentration is 5%~60% sodium alginate soln B；Third walks, and gained sodium alginate soln B is stood 2h~120h, is self-assembled into sodium alginate nano fiber；The sodium alginate of above-mentioned macromolecule refers to sodium alginate of the weight average molecular weight in 313kDa~586kDa；The sodium alginate of above-mentioned small-molecular-weight refers to the sodium alginate that weight average molecular weight is 23kDa~96kDa.
- 2. the method according to claim 1 that nanofiber is self-assembled into using small-molecular-weight sodium alginate, feature are existed In a diameter of 50nm~800nm of obtained sodium alginate nano fiber, length is 3000nm~20000nm.
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