CN107829161A - The preparation method of keratin multi-walled carbon nanotube composite fibre - Google Patents
The preparation method of keratin multi-walled carbon nanotube composite fibre Download PDFInfo
- Publication number
- CN107829161A CN107829161A CN201711209807.6A CN201711209807A CN107829161A CN 107829161 A CN107829161 A CN 107829161A CN 201711209807 A CN201711209807 A CN 201711209807A CN 107829161 A CN107829161 A CN 107829161A
- Authority
- CN
- China
- Prior art keywords
- keratin
- preparation
- walled carbon
- composite fibre
- carbon nanotube
- 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.)
- Pending
Links
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
- 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
- D01F4/00—Monocomponent artificial filaments or the like of proteins; Manufacture thereof
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Textile Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The present invention relates to synthetic fiber industry technical field, and in particular to a kind of preparation method of keratin multi-walled carbon nanotube composite fibre.A kind of preparation method of keratin multi-walled carbon nanotube composite fibre, comprises the following steps：（1）The extraction of wool keratin；（2）The preparation of function multi-walled carbon nano-tube；（3）The preparation of keratin carbon nano tube composite fibre.CNT of the present invention adds to be increased to the crystallinity of fiber, and keratin can be induced to be internally formed the secondary structure conformation of more β-pleated sheet；With the addition of CNT, the tensile break strength increase of composite fibre.
Description
Technical field
The present invention relates to synthetic fiber industry technical field, and in particular to a kind of compound fibre of keratin-multi-walled carbon nanotube
The preparation method of dimension.
Background technology
As the 2nd big wool producing country in the world, production of wool is growing, there is substantial amounts of coarse wool inferior every year in China
Gone out of use with waste and old wool product.More than 80% material is keratin in wool, and keratin has as a kind of biomaterial
Good biocompatibility and degradability, has attracted the concern of domestic and international researcher.The relative molecular mass of wool keratin
, can be as a kind of good biological spinning material mouth more than 100000.At present both at home and abroad on dissolving wool extraction keratin
Method is a lot, mainly there is reducing process, oxidizing process, ionic liquid etc..But because extraction process is complicated, post processing needs these methods
Dialysed so that whole flow process is time-consuming longer, is not easy fast and effeciently to extract keratin from wool.Therefore it is how high
Effect, rapidly dissolving wool extraction keratin are the keys to waste wool regeneration.CNT (CNTs) is used as a kind one
Dimension material has excellent mechanical property, may be used as preparing the reinforcer of high-performance composite materials, but due to CNTs major diameters
It is bigger, it is easily reunited in the base, cause enhancing effect not reach expected effect.CNTs, which is modified, to be changed
It is apt to its dispersive property, reaches good enhancing effect.Traditional acidification can damage to CNTs structures so that its performance
Weaken, and under polyphosphoric acids/phosphorus pentoxide weak acid system, losslessization is carried out to CNT by Friedel-Crafts reaction and is modified.
In its surface grafting fragrant amido group, reach dispersed purpose.
The content of the invention
It is contemplated that in view of the above-mentioned problems, propose a kind of preparation method of keratin-multi-walled carbon nanotube composite fibre.
Technical program of the present invention lies in：
A kind of preparation method of keratin-multi-walled carbon nanotube composite fibre, comprises the following steps：
（1）The extraction of wool keratin；
（2）The preparation of function multi-walled carbon nano-tube；
（3）The preparation of keratin-carbon nano tube composite fibre.
The process of the extraction of described wool keratin is：It will shred to length about 0.5cm, take after wool cleaning, drying
The g of wool 10.0,8 mol/L urea liquid, Cys 1g are placed in 500 mL three-necked flask, are adjusted with NaOH solution
PH value is saved to the h of mechanic whirl-nett reaction 24 at 11,70 DEG C, products therefrom is centrifuged and takes supernatant liquor, uses 1
Mol/L HCl solution adjusts clear liquid pH value to 4, separates out milky keratin, keratin is carried out into filtering and washing, done at 50 DEG C
It is dry to produce keratin.
The preparation method of described function multi-walled carbon nano-tube is：First, wall carbon nano tube 1g, p-aminobenzoic acid are taken
1g, polyphosphoric acids 40g are placed in 250 mL three-necked flask, are warming up to the h of mechanical agitation 3 at 130 DEG C, add phosphorus pentoxide
10g, keep 130 DEG C, the h of successive reaction 72, nitrogen protection；Products therefrom distilled water and ammoniacal liquor washing and filtering, and right repeatedly
Product distilled water and each 3d of absolute methanol surname extraction, to remove unnecessary reactant and impurity, are then dried in vacuo and produce
Function multi-walled carbon nano-tube.
The described pH value that is added to function multi-walled carbon nano-tube is 9.5, and the sodium carbonate that concentration is 0.3 mol/L buffers
1 h of ultrasound is carried out in solution, makes CNTs dispersed in the solution, keratin is then added and becomes the spinning that concentration is 20%
Silk liquid simultaneously adds the SDS that keratin mass fraction is 10%, and spinning solution is stood into 24 h is completely dissolved keratin, is subsequently heated
Continue 1 h to 90 DEG C；The preparation of composite fibre is carried out using wet spinning device, the acetic acid solution for preparing 10% is used as solidification
Bath, coagulating tank length is 1m, and spinnerette diameters are 0.13 mm, spinning speed 0.3m/min, winding speed 3m/min；
Spun composite fibre is dispelled into salt and solvent through washing, produces keratin-multi-walled carbon nanotube composite fibre.
The technical effects of the invention are that：
CNT of the present invention adds to increase to the crystallinity of fiber, and it is more that keratin can be induced to be internally formed
The secondary structure conformation of beta sheet；With the addition of CNT, the tensile break strength increase of composite fibre.
Embodiment
A kind of preparation method of keratin-multi-walled carbon nanotube composite fibre, comprises the following steps：
（1）The extraction of wool keratin：
It will be shredded after wool cleaning, drying to length about 0.5cm, take the g of wool 10.0,8 mol/L urea liquid, the Guangs of L- half
Propylhomoserin 1g is placed in 500 mL three-necked flask, and pH value is adjusted to the h of mechanic whirl-nett reaction 24 at 11,70 DEG C with NaOH solution,
Products therefrom is centrifuged and takes supernatant liquor, clear liquid pH value is adjusted to 4 using 1 mol/L HCl solution, separates out milky white
Color keratin, keratin is subjected to filtering and washing, keratin is drying to obtain at 50 DEG C.
（2）The preparation of function multi-walled carbon nano-tube：
First, take wall carbon nano tube 1g, p-aminobenzoic acid 1g, polyphosphoric acids 40g to be placed in 250 mL three-necked flask, heat up
The h of mechanical agitation 3 to 130 DEG C, phosphorus pentoxide 10g is added, keep 130 DEG C, the h of successive reaction 72, nitrogen protection；Gained produces
Thing distilled water and ammoniacal liquor washing and filtering, and to product distilled water and each 3d of absolute methanol surname extraction repeatedly, to remove
Unnecessary reactant and impurity, is then dried in vacuo and produces function multi-walled carbon nano-tube.
（3）The preparation of keratin-carbon nano tube composite fibre：
The described pH value that is added to function multi-walled carbon nano-tube is 9.5, and concentration is 0.3 mol/L sodium carbonate buffer
Middle progress 1 h of ultrasound, makes CNTs dispersed in the solution, then adds keratin and becomes the spinning solution that concentration is 20%
And the SDS that keratin mass fraction is 10% is added, spinning solution is stood into 24 h is completely dissolved keratin, is subsequently heated to 90
DEG C continue 1 h；The preparation of composite fibre is carried out using wet spinning device, the acetic acid solution for preparing 10% is used as coagulating bath, solidifying
Gu bath length is 1m, spinnerette diameters are 0.13 mm, spinning speed 0.3m/min, winding speed 3m/min；It will spin
Composite fibre through washing dispel salt and solvent, produce keratin-multi-walled carbon nanotube composite fibre.
Claims (4)
- A kind of 1. preparation method of keratin-multi-walled carbon nanotube composite fibre, it is characterised in that：Comprise the following steps：（1）The extraction of wool keratin；（2）The preparation of function multi-walled carbon nano-tube；（3）The preparation of keratin-carbon nano tube composite fibre.
- 2. the preparation method of keratin according to claim 1-multi-walled carbon nanotube composite fibre, it is characterised in that：Institute The process of the extraction for the wool keratin stated is：To be shredded after wool cleaning, drying to length about 0.5cm, take the g of wool 10.0, 8 mol/L urea liquid, Cys 1g is placed in 500 mL three-necked flask, and pH value is adjusted to 11 with NaOH solution, The h of mechanic whirl-nett reaction 24, products therefrom is centrifuged and takes supernatant liquor at 70 DEG C, uses 1 mol/L HCl solution Clear liquid pH value is adjusted to 4, milky keratin is separated out, keratin is subjected to filtering and washing, keratin is drying to obtain at 50 DEG C.
- 3. the preparation method of keratin according to claim 2-multi-walled carbon nanotube composite fibre, it is characterised in that：Institute The preparation method for the function multi-walled carbon nano-tube stated is：First, wall carbon nano tube 1g, p-aminobenzoic acid 1g, poly phosphorus are taken Sour 40g is placed in 250 mL three-necked flask, is warming up to the h of mechanical agitation 3 at 130 DEG C, adds phosphorus pentoxide 10g, is kept 130 DEG C, the h of successive reaction 72, nitrogen protection；Products therefrom distilled water and ammoniacal liquor washing and filtering, and being steamed to product repeatedly Distilled water and each 3d of absolute methanol surname extraction, to remove unnecessary reactant and impurity, then it is dried in vacuo that to produce functionalization more Wall carbon nano tube.
- 4. the preparation method of keratin according to claim 3-multi-walled carbon nanotube composite fibre, it is characterised in that：Institute The pH value that is added to function multi-walled carbon nano-tube stated is 9.5, and concentration is to be carried out in 0.3 mol/L sodium carbonate buffer 1 h of ultrasound, makes CNTs dispersed in the solution, then adds keratin and becomes the spinning solution and addition that concentration is 20% Keratin mass fraction is 10% SDS, and spinning solution is stood into 24 h is completely dissolved keratin, is subsequently heated to 90 DEG C and continues 1 h；The preparation of composite fibre is carried out using wet spinning device, prepares 10% acetic acid solution as coagulating bath, coagulating tank Length is 1m, and spinnerette diameters are 0.13 mm, spinning speed 0.3m/min, winding speed 3m/min；Will be spun compound Fiber dispels salt and solvent through washing, produces keratin-multi-walled carbon nanotube composite fibre.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711209807.6A CN107829161A (en) | 2017-11-28 | 2017-11-28 | The preparation method of keratin multi-walled carbon nanotube composite fibre |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711209807.6A CN107829161A (en) | 2017-11-28 | 2017-11-28 | The preparation method of keratin multi-walled carbon nanotube composite fibre |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107829161A true CN107829161A (en) | 2018-03-23 |
Family
ID=61645925
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201711209807.6A Pending CN107829161A (en) | 2017-11-28 | 2017-11-28 | The preparation method of keratin multi-walled carbon nanotube composite fibre |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107829161A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112062975A (en) * | 2020-09-07 | 2020-12-11 | 浙江理工大学 | Preparation method and cleaning device of regenerated wool keratin nanofiber hydrogel |
-
2017
- 2017-11-28 CN CN201711209807.6A patent/CN107829161A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112062975A (en) * | 2020-09-07 | 2020-12-11 | 浙江理工大学 | Preparation method and cleaning device of regenerated wool keratin nanofiber hydrogel |
| CN112062975B (en) * | 2020-09-07 | 2023-05-26 | 浙江理工大学 | Preparation method and cleaning device of regenerated wool keratin nanofiber hydrogel |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102102233B (en) | Method for preparing polyacrylonitrile-based carbon nanofiber precursor | |
| Celebioglu et al. | Cyclodextrin nanofibers by electrospinning | |
| CN103061174B (en) | The method preparing cellulose nanometer fibril is assisted in a kind of strong acid preliminary treatment | |
| JP7368923B2 (en) | Method for producing carbon fibers from recycled cotton and use of the fibers obtained by this method for forming articles from composite materials | |
| CN103031611B (en) | A kind of vinal and its preparation method and application | |
| CN106906531A (en) | The preparation method of Graphene fibroin protein functional fiber | |
| CN107177892B (en) | A kind of core-shell structure fiber and preparation method thereof based on carbon nanomaterial | |
| CN111155217A (en) | Method for improving orientation degree and conductivity of carbon nanotube fibers | |
| CN104264263A (en) | Fibroin/carbon nano tube hybridization fiber and preparation method thereof | |
| CN104947244A (en) | Method for extracting and preparing lignin composite nano fibers in situ | |
| CN106757538A (en) | A kind of electrical spinning method prepares porous carbon fiber preparation method | |
| CN104975368A (en) | Multiwalled carbon nanotube and graphene reinforced modified regenerated protein fiber and preparation method thereof | |
| CN101550610A (en) | Preparation method of chitosan fiber | |
| CN103102694A (en) | Method for preparation and wet spinning of regenerative keratin and silk-fibroin blended solution | |
| CN106637480A (en) | Preparation method of high-shrinkage fiber | |
| CN104878465A (en) | Carbon nanotube regenerated bamboo fibers and production method therefor | |
| CN103215683A (en) | Preparation method of carbon nanotube-reinforced polyvinyl alcohol composite fiber | |
| CN103668616B (en) | A kind of carbon nano-tube modification polyvinyl alcohol nano yarn and preparation method thereof | |
| CN101230495A (en) | Solvent preparation of cellulose fiber releasing anion and use thereof | |
| Li et al. | Fabrication and performance of wool keratin–functionalized graphene oxide composite fibers | |
| CN103668528B (en) | A kind of carbon nanotube/polyvinyl alcohol composite fibre and preparation method thereof | |
| CN107829161A (en) | The preparation method of keratin multi-walled carbon nanotube composite fibre | |
| CN103526330A (en) | Strain-sensing nano fiber yarn and preparation method thereof | |
| CN114163684A (en) | Method for directly extracting fibroin nanofibers from waste silkworm cocoons and recovering hydrolyzed silk protein and extracting solution | |
| CN117431660A (en) | Method for preparing functional keratin fibers by using waste wool |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| WD01 | Invention patent application deemed withdrawn after publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20180323 |