CN107794601B - Spinning solution for preparing high-algae-content nano fibers and application thereof - Google Patents
Spinning solution for preparing high-algae-content nano fibers and application thereof Download PDFInfo
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- CN107794601B CN107794601B CN201710814564.2A CN201710814564A CN107794601B CN 107794601 B CN107794601 B CN 107794601B CN 201710814564 A CN201710814564 A CN 201710814564A CN 107794601 B CN107794601 B CN 107794601B
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- 238000009987 spinning Methods 0.000 title claims abstract description 65
- 239000002121 nanofiber Substances 0.000 title claims abstract description 36
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims abstract description 36
- -1 polyoxyethylene Polymers 0.000 claims abstract description 35
- 238000000034 method Methods 0.000 claims abstract description 26
- 241001474374 Blennius Species 0.000 claims abstract description 25
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000008367 deionised water Substances 0.000 claims abstract description 14
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 14
- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 claims abstract description 9
- 235000010413 sodium alginate Nutrition 0.000 claims abstract description 9
- 239000000661 sodium alginate Substances 0.000 claims abstract description 9
- 229940005550 sodium alginate Drugs 0.000 claims abstract description 9
- FHVDTGUDJYJELY-UHFFFAOYSA-N 6-{[2-carboxy-4,5-dihydroxy-6-(phosphanyloxy)oxan-3-yl]oxy}-4,5-dihydroxy-3-phosphanyloxane-2-carboxylic acid Chemical compound O1C(C(O)=O)C(P)C(O)C(O)C1OC1C(C(O)=O)OC(OP)C(O)C1O FHVDTGUDJYJELY-UHFFFAOYSA-N 0.000 claims description 17
- 229940072056 alginate Drugs 0.000 claims description 17
- 229920000615 alginic acid Polymers 0.000 claims description 17
- 235000010443 alginic acid Nutrition 0.000 claims description 17
- 238000003756 stirring Methods 0.000 claims description 5
- 230000008569 process Effects 0.000 abstract description 8
- 241000195493 Cryptophyta Species 0.000 abstract description 6
- 238000002360 preparation method Methods 0.000 abstract description 6
- 238000005516 engineering process Methods 0.000 abstract description 4
- 239000012467 final product Substances 0.000 abstract description 3
- 239000002904 solvent Substances 0.000 abstract description 3
- 239000006184 cosolvent Substances 0.000 abstract description 2
- 230000006872 improvement Effects 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 239000000047 product Substances 0.000 abstract description 2
- 239000004094 surface-active agent Substances 0.000 abstract description 2
- 239000000835 fiber Substances 0.000 description 32
- 238000010041 electrostatic spinning Methods 0.000 description 7
- 238000001000 micrograph Methods 0.000 description 6
- 229920001282 polysaccharide Polymers 0.000 description 5
- 229920000945 Amylopectin Polymers 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 230000002349 favourable effect Effects 0.000 description 3
- 239000002105 nanoparticle Substances 0.000 description 3
- 238000001878 scanning electron micrograph Methods 0.000 description 3
- 230000007547 defect Effects 0.000 description 2
- 238000001523 electrospinning Methods 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000004753 textile Substances 0.000 description 2
- 230000009471 action Effects 0.000 description 1
- 239000002671 adjuvant Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000003995 emulsifying agent Substances 0.000 description 1
- 150000004676 glycans Chemical class 0.000 description 1
- 230000003340 mental effect Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 239000000825 pharmaceutical preparation Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000005017 polysaccharide Substances 0.000 description 1
- APTZNLHMIGJTEW-UHFFFAOYSA-N pyraflufen-ethyl Chemical compound C1=C(Cl)C(OCC(=O)OCC)=CC(C=2C(=C(OC(F)F)N(C)N=2)Cl)=C1F APTZNLHMIGJTEW-UHFFFAOYSA-N 0.000 description 1
- 238000004513 sizing Methods 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 238000002560 therapeutic procedure Methods 0.000 description 1
- 239000002562 thickening agent Substances 0.000 description 1
Images
Classifications
-
- 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
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/18—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from other substances
-
- 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
- D01D1/00—Treatment of filament-forming or like material
- D01D1/02—Preparation of spinning solutions
-
- 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
- D01D5/18—Formation of filaments, threads, or the like by means of rotating spinnerets
-
- 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
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
- D01F8/16—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one other macromolecular compound obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds as constituent
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- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Mechanical Engineering (AREA)
- Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Artificial Filaments (AREA)
- Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)
Abstract
The invention relates to the field of nanofiber preparation, and aims to provide a spinning solution for preparing nanofibers with high seaweed content and application thereof. The spinning solution consists of sodium alginate, polyoxyethylene and deionized water; wherein the mass percentage of the sodium alginate is 2.5-3.5%, the mass percentage of the polyoxyethylene is 0.1-0.3%, and the balance is deionized water. The invention utilizes deionized water as a solvent to prepare spinning solution, and the spinning solution does not contain any surfactant and cosolvent, thereby preparing the nanofiber with high algae content by utilizing a centrifugal spinning technology. The invention can realize the remarkable improvement of the quality of the seaweed nano fiber by only using a very small amount of polyoxyethylene, and the percentage content of the seaweed in the final product is higher than 89%. The obtained seaweed nano-fiber has good compatibility with ecological environment, is biodegradable, is a novel green product, has very wide market prospect, and can be used in the fields of novel medical dressings and the like. Simple process and high production efficiency.
Description
Technical Field
The invention belongs to the field of nanofiber preparation, and relates to a spinning solution for preparing high-algae-content nanofibers and application thereof.
Background
Alginate is a natural polysaccharide, and has the stability, solubility, viscosity and safety required by pharmaceutical preparation adjuvants. At present, sodium alginate is mainly used as a sizing agent and a printing paste of textiles, and is simultaneously used as a thickening agent, a stabilizing agent and an emulsifying agent in the food industry. With the proposal of the wet therapy, the alginate fiber has great application prospect in the field of novel medical textiles due to excellent bacteriostasis, high hygroscopicity, high oxygen permeability, gel flame retardance, biodegradability and biocompatibility.
Now, the conventional alginate fiber is mainly wet-spun, the fiber diameter is in the range of tens of microns to tens of microns, and if a thinner fluffy fiber aggregate can be prepared, the application of the alginate fiber aggregate in medical dressing and the like is more advantageous.
The existing spinning method for preparing the seaweed nano fiber mainly adopts an electrostatic spinning method, but the method has two problems:
firstly, as the electrostatic spinning is to draft the spinning solution into fiber by high-voltage electrostatic force, the taylor instability phenomenon, jet thunderbolt phenomenon and the like can occur in the fiber forming process. Therefore, the process has higher requirement on the spinnability of the spinning solution and needs the spinning solution to have better fiber forming property. In general, a skilled person will add a certain amount of polyoxyethylene with better fiberizability to the spinning solution to provide sufficient entanglement of molecular segments to ensure smooth spinning, and it is considered that the higher the polyoxyethylene content is, the more favorable the entanglement of molecular segments and smooth spinning are. Based on this knowledge, in the spinning solution in which alginate, polyoxyethylene and deionized water are mixed, the mass percentage of polyoxyethylene accounts for more than 30% of the total solute mass (i.e. the mass ratio of alginate to polyoxyethylene is less than 7: 3). If the mass percentage of polyoxyethylene accounts for less than 30% of the total solute mass (i.e., the mass ratio of alginate to polyoxyethylene is greater than 7:3), fibers cannot be spun smoothly. Thus, the seaweed content in the prepared seaweed Nanofibers usually cannot exceed 70% by weight (Saving C D, Tang C, Monian B, et al, Alginate-Polyethylene Oxide Blend Nanofibers and the Role of the carrier Polymer in electrochemical research [ J ]. Industrial & Engineering chemistry research,2013,52(26): 8692-.
Secondly, due to the electrostatic action, the final product can only be a compact film, if a fiber aggregate with a loose structure needs to be prepared, the fiber aggregate can only be formed through centrifugal spinning, and the electrostatic spinning method has the defect of extremely low yield, so that the industrialization is difficult to realize.
Centrifugal spinning is a method that has emerged in recent years that can be used to produce nanofibers, the principle of which is: the spinning solution overcomes viscous force and surface tension in a spinning nozzle rotating at high speed to form jet flow which is sprayed out from the spinning nozzle, and the jet flow is solidified into fiber in the process of stretching and thinning. However, if the spinning solution in the electrospinning method is directly used for centrifugal spinning, there is a problem that the seaweed content in the final fiber is less than 70%. In the electrospinning method, in order to provide sufficient molecular chain entanglement to ensure smooth spinning, the mass percentage of polyoxyethylene must account for more than 30% of the total solute mass (i.e. the mass ratio of alginate to polyoxyethylene is less than 7:3), and it is well known in the industry that the higher the mass percentage of polyoxyethylene, the more favorable the spinning is. At present, when various fibers are prepared by centrifugal spinning, the proportion of spinning solution is carried out by referring to electrostatic spinning solution, and the fibers can be prepared smoothly, but the problem of low content of main components in the fibers is also existed.
Disclosure of Invention
The invention aims to solve the technical problem of overcoming the defects in the prior art and provides a spinning solution for preparing high-algae-content nano fibers and application thereof.
In order to realize the purpose of the invention, the technical scheme adopted by the invention is as follows:
providing a spinning solution for preparing high-seaweed-content nano fibers, wherein the spinning solution consists of sodium alginate, polyoxyethylene and deionized water; wherein the mass percentage of the sodium alginate is 2.5-3.5%, the mass percentage of the polyoxyethylene is 0.1-0.3%, and the balance is deionized water.
The invention further provides a method for preparing the high-algae-content nano-fiber by using the spinning solution, which comprises the steps of mixing alginate, polyoxyethylene and deionized water according to the proportion at room temperature, uniformly stirring, and carrying out vacuum defoaming treatment; and the prepared spinning solution is used for preparing the nano-fiber with high alga content by a centrifugal spinning method.
Description of the inventive principles:
currently, in the electrostatic spinning method, in the spinning solution formed by mixing alginate, polyoxyethylene and deionized water, the mass percentage of polyoxyethylene must account for more than 30% of the total solute mass (i.e. the mass ratio of alginate to polyoxyethylene is less than 7: 3). The theoretical basis is as follows: the polyoxyethylene has better fiber forming property, can provide enough entanglement of molecular chain segments to ensure smooth spinning, and the higher the polyoxyethylene content is, the more favorable the entanglement of the molecular chain segments and the smooth spinning are. Therefore, in order to make the spinning dope fiberizable, it is necessary to add a sufficient amount of polyoxyethylene to the spinning dope. Such practice has become a common practice in the industry and has even led to a mental position for the understanding of the technology. At present, when various fibers are prepared by centrifugal spinning, the proportion of spinning solution is carried out by referring to electrostatic spinning solution, and the fibers can be prepared smoothly, but the problem of low content of main components in the fibers is also existed.
For alginate fibers, polyoxyethylene is added in electrostatic spinning to improve spinnability by utilizing the entanglement effect between the polyoxyethylene and alginate molecular chains, but the effect can be achieved only by using a certain amount of polyoxyethylene content. The inventor has found that in the centrifugal spinning process, under the condition of low content, polyoxyethylene does not play a role in providing molecular chain segment entanglement in the spinning solution, but forms hydrogen bonds with seaweed molecules, so that the acting force between the seaweed and water molecules is weakened, and the water solvent can be volatilized in time in the spinning process to promote the formation of fibers. Therefore, the centrifugal spinning method can improve the spinnability by utilizing the hydrogen bonding effect between the polyoxyethylene and the seaweed, and the smooth spinning can be ensured only by adding a small amount of polyoxyethylene. Thereby greatly reducing the content of polyoxyethylene.
Compared with the prior art, the invention has the beneficial effects that:
(1) the invention provides a new green technology for preparing high-algae-content nano-fibers, which is to prepare spinning solution by using deionized water as a solvent, wherein the spinning solution does not contain any surfactant and cosolvent, and then prepare the high-algae-content nano-fibers by using a centrifugal spinning technology.
(2) The invention can realize the remarkable improvement of the quality of the seaweed nano fiber by using only a very small amount of polyoxyethylene. In the final product, the percentage of seaweed is higher than 89%, up to 96.8%.
(3) The invention has simple process and high production efficiency.
(4) The seaweed nano-fiber obtained by the preparation method has good compatibility with ecological environment, is biodegradable, is a novel green product, has very wide market prospect, and can be used in the fields of novel medical dressings and the like.
Drawings
FIG. 1 is a scanning electron microscope image of the nano-sized algae fiber prepared in example 1 of the present invention, magnified twenty thousand times.
FIG. 2 is a scanning electron microscope image of the nano-sized algae fiber prepared in example 1 of the present invention, at a magnification of five hundred times.
FIG. 3 is a scanning electron microscope image of the nano-fiber of seaweed prepared in example 2 of the present invention with a magnification of twenty thousand times.
FIG. 4 is a scanning electron microscope image of the marine algae nanofibers prepared in example 2 of the present invention at a magnification of five hundred times.
FIG. 5 is a scanning electron microscope image of the nano-sized algae fiber prepared in example 3 of the present invention, magnified twenty thousand times.
FIG. 6 is a scanning electron microscope image of the marine algae nanofibers prepared in example 3 of the present invention at a magnification of five hundred times.
Detailed Description
The centrifugal spinning method of the present invention can be carried out by referring to the method described in (Li X, Chen H, Yang B.Centrifuguely spun-based fibers from amylopectin rich stages [ J ]. Carbohydrate Polymers,2016,137: 459-.
Example 1:
(1) preparing spinning solution from 2.5g of sodium alginate, 0.3g of polyoxyethylene and 97.2g of deionized water, uniformly stirring, and then defoaming in vacuum;
(2) the preparation of alginate nanofibers by centrifugal spinning technique can be described in (Li X, Chen H, Yang B. Centrifugly spun-based fibers from amylopectin rich residues [ J ]. Carbohydrate Polymers,2016,137: 459-. The process conditions are as follows: the spinning speed is 2000r/min, the diameter of a spinning nozzle is 0.20mm, and the collection distance is 10 cm. FIGS. 1 and 2 are scanning electron micrographs of the prepared seaweed nanofibers. Tests show that the diameter of the prepared seaweed nano fiber is about 300nm, and the mass percentage of seaweed in the fiber is 89.3%.
Example 2:
(1) preparing spinning solution from 3.0g of sodium alginate, 0.1g of polyoxyethylene and 96.9g of deionized water, uniformly stirring, and then defoaming in vacuum;
(2) the preparation of alginate nanofibers by centrifugal spinning technique can be described in (Li X, Chen H, Yang B. Centrifugly spun-based fibers from amylopectin rich residues [ J ]. Carbohydrate Polymers,2016,137: 459-. The process conditions are as follows: the spinning speed is 2500r/min, the diameter of a spinning nozzle is 0.33mm, and the collection distance is 11 cm. FIGS. 3 and 4 are scanning electron micrographs of the prepared seaweed nanofibers. Tests show that the diameter of the prepared seaweed nano fiber is about 400nm, and the mass percentage of seaweed in the fiber is 96.8%.
Example 3:
(1) preparing spinning solution from 3.5g of sodium alginate, 0.2g of polyoxyethylene and 96.3g of deionized water, stirring uniformly, then defoaming in vacuum,
(2) the preparation of alginate nanofibers by centrifugal spinning technique can be described in (Li X, Chen H, Yang B. Centrifugly spun-based fibers from amylopectin rich residues [ J ]. Carbohydrate Polymers,2016,137: 459-. The process conditions are as follows: the spinning speed is 3500r/min, the diameter of the spinning nozzle is 0.16mm, and the collection distance is 13 cm. FIGS. 5 and 6 are scanning electron micrographs of the prepared seaweed nanofibers. Tests show that the diameter of the prepared seaweed nano fiber is about 530nm, and the mass percentage of seaweed in the fiber is 94.6%.
Claims (1)
1. A method for preparing high-algae-content nano fibers is characterized by comprising the following steps:
(1) mixing alginate, polyoxyethylene and deionized water at room temperature, stirring uniformly, and performing vacuum defoaming treatment to obtain a spinning solution; in the spinning solution, the mass percentage of sodium alginate is 2.5-3.5%, the mass percentage of polyoxyethylene is 0.1-0.3%, and the balance is deionized water;
(2) the spinning solution is used for preparing the nano-fiber by a centrifugal spinning method, and the percentage content of the seaweed in the nano-fiber product is higher than 89%.
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| CN201710814564.2A CN107794601B (en) | 2017-09-12 | 2017-09-12 | Spinning solution for preparing high-algae-content nano fibers and application thereof |
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| CN107794601B true CN107794601B (en) | 2020-01-21 |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105311001A (en) * | 2015-06-01 | 2016-02-10 | 李江涛 | VEGF (vascular endothelial growth factor)-loaded hydrogel fiber membrane for liver regeneration and preparation method thereof |
| CN105586716A (en) * | 2014-10-26 | 2016-05-18 | 天津开发区金衫包装制品有限公司 | High-content sodium alginate nanofiber membrane and electrostatic spinning manufacturing method thereof |
| CN106480517A (en) * | 2015-08-31 | 2017-03-08 | 青岛新智源健康科技有限公司 | A kind of sodium alginate nano fiber and its scale electro spinning method for preparing and application |
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2017
- 2017-09-12 CN CN201710814564.2A patent/CN107794601B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105586716A (en) * | 2014-10-26 | 2016-05-18 | 天津开发区金衫包装制品有限公司 | High-content sodium alginate nanofiber membrane and electrostatic spinning manufacturing method thereof |
| CN105311001A (en) * | 2015-06-01 | 2016-02-10 | 李江涛 | VEGF (vascular endothelial growth factor)-loaded hydrogel fiber membrane for liver regeneration and preparation method thereof |
| CN106480517A (en) * | 2015-08-31 | 2017-03-08 | 青岛新智源健康科技有限公司 | A kind of sodium alginate nano fiber and its scale electro spinning method for preparing and application |
Non-Patent Citations (2)
| Title |
|---|
| Centrifugally spun starch-based fibers from amylopectin rich starches;Li X.et al.;《Carbohydrate Polymers》;20161231;459-465 * |
| Electrospun Sodium Alginate/Polyethylene Oxide Fibers and Nanocoated Yarns;C.Hu.et al.;《International Journal of Polymer Science》;20151231;1-12 * |
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