CN107287686A - A kind of electrically conductive filament and preparation method thereof - Google Patents
A kind of electrically conductive filament and preparation method thereof Download PDFInfo
- Publication number
- CN107287686A CN107287686A CN201710417544.1A CN201710417544A CN107287686A CN 107287686 A CN107287686 A CN 107287686A CN 201710417544 A CN201710417544 A CN 201710417544A CN 107287686 A CN107287686 A CN 107287686A
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- China
- Prior art keywords
- shell
- acid
- electrically conductive
- preparation
- conductive filament
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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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
- D01F8/02—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from cellulose, cellulose derivatives, or proteins
-
- 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
- D01D5/06—Wet spinning methods
-
- 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
- D01D5/12—Stretch-spinning methods
- D01D5/14—Stretch-spinning methods with flowing liquid or gaseous stretching media, e.g. solution-blowing
-
- 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
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/09—Addition of substances to the spinning solution or to the melt for making electroconductive or anti-static filaments
-
- 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
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
-
- 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)
- Manufacturing & Machinery (AREA)
- Materials For Medical Uses (AREA)
- Artificial Filaments (AREA)
Abstract
The invention discloses a kind of electrically conductive filament and preparation method thereof, belong to the technical field of bio-medical material and conductive material.The preparation method is as follows：(1) shell is subjected to pre-treatment, is prepared into solution；(2) spinning solution prepares；(3) prepared by electrically conductive filament.The present invention prepares dissolution system using waste shell as raw material, and the recycling for realizing shell is recycled, and raw materials used cheap, whole preparation process mild condition is controllable, and preparation technology is simple, can be continuously produced.
Description
Technical field
The invention belongs to silk fibre composite, conductive fiber material technical field there is provided a kind of electrically conductive filament and its
Preparation method.
Background technology
It is existing in order to improve application of the silk based composites in neural tissue engineering and artificial neuron repair materials field
Conducting polymer is compound with other high polymer materials, but these material own biological compatibilities are not enough, limit it in clinic
Application in terms of medical science.At present, there is not yet fibroin albumen and the compound report for preparing filament fiber of polyaniline.
The preparation method of electrically conductive filament mainly has：(1) conductive compositions, this method materials conductive are coated on conventional fibre surface
Performance is protruded, but poor durability；(2) conductive material is made with fibrous raw material blending, conductive particle in material prepared by this method
It is sub easily to reunite, influence materials conductive effect.
It is currently reported that polyaniline is prepared into conductive fiber, Chinese invention patent " polyaniline nano fiber and its system
Polyaniline and ferric pyrophosphate are dissolved in inorganic acid by Preparation Method " respectively, mixing, filter, be dried to obtain polyaniline nano fiber.In
Conductive fiber is made in polyaniline master batch melt-spraying spinning by state's patent of invention " a kind of preparation method of Conductive Polyaniline Fibers ".China
Patent of invention " a kind of preparation method of the controllable polyaniline film in aperture " prepares porous polyaniline using electrochemical polymerization
Film.Chinese invention patent " a kind of bionical regenerated silk fibroin filament fiber and preparation method thereof " uses wet method or dry spinning
Prepare fibroin albumen filament fiber.Zhang Jianguang etc. prepares orientation polyaniline/fibroin albumen composite Nano using electrostatic spinning technique
Fiber, for fields such as nerve regneration, osteanagenesis, (Zhang Jianfei, Sun Binbin, show plum Static Spinnings polyaniline/fibroin albumen is not compound
The 29th Annual Conference summary collection of preparation and its sign Chinese Chemical Societys of nanofiber, 2014).
The content of the invention
The problem of for existing artificial neuron repair materials biocompatibility deficiency, it is an object of the present invention to provide a kind of conductive
Long filament and preparation method thereof.
To reach above-mentioned purpose, the technical solution adopted by the present invention is：A kind of electrically conductive filament and preparation method thereof, including such as
Lower step：
(1) shell is cleaned, dried, crushed, ground, obtain powder particle, powder particle is dissolved in acid system, prepared
Into shell-acid dissolution system.
(2) by boiled silk and polyaniline with mass ratio 99:1-80:20 are dissolved in shell-acid dissolution system, and stirring is equal
It is even, it is prepared into spinning solution.
(3) high water absorption that the aqueous solutions of organic solvent or mass fraction for being 0%-100% with mass fraction are 0%-90%
Property the material aqueous solution be prepared into coagulating bath, spinning solution is put into device for spinning, wet spinning/dry is then carried out in coagulating bath
Wet spinning, cleaning obtains just growing filament.
(4) high water absorption that the aqueous solutions of organic solvent or mass fraction for being 0%-100% with mass fraction are 0%-90%
Property the material aqueous solution be prepared into drawing-off bath, by first growing filament drawing-off bath in carry out once or more drawing-off, led
Electric filament fiber.
In above-mentioned technical proposal, the shell is one kind in the shells such as pearl shell, scallop shell, CONCHA MERETRICID SEU CYCLINAE, conch shell
Or it is a variety of.
In above-mentioned technical proposal, acid is in formic acid, hydrochloric acid, acetic acid, phosphoric acid, sulfuric acid in the shell-acid dissolution system
One or more, acid concentration is 30%-100%.
In above-mentioned technical proposal, organic solvent is ethanol, methanol etc. in coagulating bath and the drawing-off bath；High-hydroscopicity material
For polyethylene glycol, ammonium sulfate etc..
Because above-mentioned technical proposal is used, the present invention has following advantages compared with prior art：
(1) present invention prepares dissolution system by raw material of shell and is used to prepare electrically conductive filament material, and shell is realized first
Recycling is recycled, meanwhile, the also preparation for fibroin albumen base regrown material provides new method.
(2) preparation process mild condition disclosed by the invention is controllable, and preparation technology is simple, the filamentary material biofacies of preparation
Capacitive is good, can be in biomedical sector application.
Brief description of the drawings
The scanning electron microscope (SEM) photograph of the electrically conductive filament of accompanying drawing 1
Embodiment
With reference to embodiment, the invention will be further described：
Embodiment one
A kind of electrically conductive filament and preparation method thereof, comprises the following steps：
(1) oyster shell is cleaned, dried, crushed, grind, sieved, obtain the shell powder that particle diameter is less than 1 μm.
(2) 0.5g shell powders are dissolved in 9.5g formic acid solutions, are prepared into formic acid/shell that mass fraction is 5%
Dissolution system.
(3) 1.0g fibroin albumens silk, 0.5g polyanilines are added in formic acid/shell dissolution system, 2h is stirred at room temperature, made
It is standby into spinning solution.
(4) ethanol solution that mass fraction is 75% is prepared as coagulating bath, spinning solution is injected in syringe, using wet
Method spinning prepares just growing filament.
(5) first growing filament is immersed in 60 DEG C of deionized waters and carries out 1 times, 2 times and 3 times drawing-off respectively.
(6) it will be batched by the long filament after the completion of drawing-off with 60 meters per minute of speed, obtain fibroin albumen/polyaniline and lead
Electric long filament.
Embodiment two
A kind of electrically conductive filament and preparation method thereof, comprises the following steps：
(1) oyster shell is cleaned, dried, crushed, grind, sieved, obtain the shell powder that particle diameter is less than 1 μm.
(2) 10g shell powders are dissolved in 90g formic acid solutions, are prepared into formic acid/shell that mass fraction is 10% molten
Enzymatic hydrolysis system.
(3) 20g fibroin albumens silk, 5g polyanilines are added in formic acid/shell dissolution system, 6h is stirred at room temperature, prepared
Into spinning solution.
(4) ammonium sulfate that mass fraction is 60% is prepared as coagulating bath, and spinning solution is injected in syringe, used
Wet spinning prepares just growing filament.
(5) drawing-off bath uses mass fraction for 20% ethanol solution, and first growing filament is immersed in 60 DEG C of drawing-off baths respectively
Carry out 1 times, 2 times and 3 times drawing-off.
(6) it will be batched by the long filament after the completion of drawing-off with 30 meters per minute of speed, obtain fibroin albumen/polyaniline and lead
Electric long filament.
Embodiment three
A kind of electrically conductive filament and preparation method thereof, comprises the following steps：
(1) CONCHA MERETRICID SEU CYCLINAE is cleaned, dried, crushed, grind, sieved, obtain the shell powder that particle diameter is less than 10 μm.
(2) 5g shell powders are dissolved in 95g phosphoric acid solutions, are prepared into phosphoric acid/shell dissolving that mass fraction is 5%
System.
(3) 30g fibroin albumens silk, 3.3g polyanilines are added in phosphoric acid/shell dissolution system, 8h is stirred at room temperature, made
It is standby into spinning solution.
(4) methanol solution that mass fraction is 50% is prepared as coagulating bath, spinning solution is injected in syringe, using dry
Wet spinning prepares just growing filament.
(5) first growing filament is immersed into mass fraction to lead to carry out 1 times, 3 times and 5 times respectively in 10% polyglycol solution
Stretch.
(6) it will be batched by the long filament after the completion of drawing-off with 10 meters per minute of speed, obtain fibroin albumen/polyaniline and lead
Electric long filament.
Example IV
A kind of electrically conductive filament and preparation method thereof, comprises the following steps：
(1) pearl shell is cleaned, dried, crushed, grind, sieved, obtain the shell powder that particle diameter is less than 10 μm.
(2) 2g shell powders are dissolved in 18g phosphoric acid solutions, are prepared into phosphoric acid/shell that mass fraction is 10% molten
Enzymatic hydrolysis system.
(3) 5g fibroin albumens silk, 0.1g polyanilines are added in phosphoric acid/shell dissolution system, 6h is stirred at room temperature, prepared
Into spinning solution.
(4) ammonium sulfate that mass fraction is 80% is prepared as coagulating bath, and spinning solution is injected in syringe, used
Dry-wet spinning prepares just growing filament.
(5) drawing-off bath uses mass fraction for 40% ethanol solution, will carry out 1 respectively in the immersion drawing-off bath of first growing filament
Again with 3 times of drawing-offs.
(6) it will be batched by the long filament after the completion of drawing-off with 10 meters per minute of speed, obtain fibroin albumen/polyaniline and lead
Electric long filament.
Claims (6)
1. a kind of electrically conductive filament and preparation method thereof, it is characterised in that described electrically conductive filament is main by fibroin albumen and polyphenyl
Amine is constituted.The filament diameter is 1-500 μm, and tensile break strength is 1MPa-1GPa under dry state, and elongation at break is
0.01%-90%.
2. a kind of electrically conductive filament according to claim 1 and preparation method thereof, it is characterised in that comprise the following steps：
(1) shell is cleaned, dried, crushed, ground, obtain powder particle, powder particle is dissolved in acid system, is prepared into shellfish
Shell-acid dissolution system.
(2) by boiled silk and polyaniline with mass ratio 99:1-80:20 are dissolved in shell-acid dissolution system, stir, system
It is standby into spinning solution.
(3) the high-hydroscopicity thing that the aqueous solutions of organic solvent or mass fraction for being 0%-100% with mass fraction are 0%-90%
The matter aqueous solution is prepared into coagulating bath, and spinning solution is put into device for spinning, and wet spinning/wet-dry change is then carried out in coagulating bath
Spinning, cleaning obtains just growing filament.
(4) the high-hydroscopicity thing that the aqueous solutions of organic solvent or mass fraction for being 0%-100% with mass fraction are 0%-90%
The matter aqueous solution is prepared into drawing-off bath, and first growing filament is carried out to the drawing-off of once or more in drawing-off bath, conductive length is obtained
Silk fiber.
3. a kind of electrically conductive filament according to claim 2 and preparation method thereof, it is characterised in that：The shell is pearl shell
One or more in the shells such as shell, scallop shell, CONCHA MERETRICID SEU CYCLINAE, conch shell.
4. a kind of electrically conductive filament according to claim 2 and preparation method thereof, it is characterised in that：The shell-acid dissolving
Acid is the one or more in formic acid, hydrochloric acid, acetic acid, phosphoric acid, sulfuric acid in system, and acid concentration is 30%-100%.
5. a kind of electrically conductive filament according to claim 2 and preparation method thereof, it is characterised in that：The coagulating bath and drawing-off
Organic solvent is ethanol, methanol etc. in bath；High-hydroscopicity material is polyethylene glycol, ammonium sulfate etc..
6. the electrically conductive filament material prepared as the method described in claim 2,3,4,5.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710417544.1A CN107287686A (en) | 2017-06-06 | 2017-06-06 | A kind of electrically conductive filament and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710417544.1A CN107287686A (en) | 2017-06-06 | 2017-06-06 | A kind of electrically conductive filament and preparation method thereof |
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| Publication Number | Publication Date |
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| CN107287686A true CN107287686A (en) | 2017-10-24 |
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| CN201710417544.1A Pending CN107287686A (en) | 2017-06-06 | 2017-06-06 | A kind of electrically conductive filament and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108042844A (en) * | 2017-12-11 | 2018-05-18 | 青岛大学 | A kind of preparation method of suture |
| CN111088528A (en) * | 2018-10-24 | 2020-05-01 | 中国石油化工股份有限公司 | Conductive spinning solution, preparation method and application of conductive acrylic fiber |
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2017
- 2017-06-06 CN CN201710417544.1A patent/CN107287686A/en active Pending
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| CN1316554A (en) * | 2001-04-29 | 2001-10-10 | 东华大学 | Electrically conductive polyphenylamine/polyamide fibre and its preparing process |
| CN101560327A (en) * | 2008-04-17 | 2009-10-21 | 中国船舶重工集团公司第七二五研究所 | Method for preparing polyaniline/nylon 66 conductive composite material |
| CN103160946A (en) * | 2011-12-13 | 2013-06-19 | 西安瑞捷生物科技有限公司 | Preparation method of tissue engineering scaffold fibrous material |
| CN103320886A (en) * | 2013-07-15 | 2013-09-25 | 苏州大学 | Bionic regenerated silk fibroin filament fiber and preparation method thereof |
| CN106637993A (en) * | 2016-12-01 | 2017-05-10 | 西南大学 | Preparation method for polyaniline conductive silk fabric |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108042844A (en) * | 2017-12-11 | 2018-05-18 | 青岛大学 | A kind of preparation method of suture |
| CN111088528A (en) * | 2018-10-24 | 2020-05-01 | 中国石油化工股份有限公司 | Conductive spinning solution, preparation method and application of conductive acrylic fiber |
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Application publication date: 20171024 |