CN107541078A - A kind of silk fibre composite of graphene oxide parcel and preparation method thereof - Google Patents
A kind of silk fibre composite of graphene oxide parcel and preparation method thereof Download PDFInfo
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- CN107541078A CN107541078A CN201710836602.4A CN201710836602A CN107541078A CN 107541078 A CN107541078 A CN 107541078A CN 201710836602 A CN201710836602 A CN 201710836602A CN 107541078 A CN107541078 A CN 107541078A
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Abstract
The invention discloses silk fibre composite of a kind of graphene oxide parcel and preparation method thereof, preparation process is as follows：Use poly-dopamine modified lithium salix cellulose；Magnetic porous composite material is obtained using liquid nitrogen, frozen dried；Magnetic porous composite material is immersed in 1 12h in graphene oxide solution, cleaned repeatedly with ethanol and deionized water after taking-up, the silk fibre composite of graphene oxide parcel is obtained after vacuum drying.The present invention uses salix monogolica and silk as base material, raw material is sufficient, it is cheap, then magnetic nano ferroferric oxide, graphene oxide are subjected to effective collaboration self assembly, the silk fibre composite of graphene oxide parcel is obtained, has potential application value in fields such as sorbing material, photocatalysis, biomaterial, medical materials.
Description
Technical field
The present invention relates to a kind of silk fibre composite of graphene oxide parcel, belongs to field of compound material.
Background technology
Silk is described as fiber queen, and its is soft, abundant, smooth, plentiful, possesses gloss soft as pearl,
Weaving, apparel industry are widely used.Silk is made up of silk gum and fibroin, and wherein silk gum is located at the outer layer of silk, content
Between 20%-30%, fibroin is located at the internal layer of silk, and content is between 70%-80%.Fibroin positioned at silk internal layer is one
Kind natural macromolecular material, by serine（serine）, glycine（Glycine）, alanine（alanine）Deng 18 kinds of amino
Acid composition, molecular weight is about 2300kDa, is made up of heavy chain, light chain and P25, and wherein the molecular weight of heavy chain H chains is 350kDa, gently
Chain L chain molecular weights are 26kDa, and P25 molecular weight is 30kDa, and the ratio of three is 6:6:1.Fibroin share 11 noncrystalline domains and
12 crystal regions, by disulfide bond between heavy chain H chains and light chain L chains, form H-L complexs.
The crystal habit of fibroin is broadly divided into two kinds of the type of fibroin I and II type of fibroin.The type of fibroin I is a kind of knot of meta-stable
Structure, conformation are crank shape or zigzag, are a kind of intermediatenesses between alpha-helix and beta sheet, and structure cell belongs to orthorhombic
System.Handled through damp and hot, sour, polar solvent etc., the type of fibroin I is easy to change to the type of fibroin II.The type of fibroin II is antiparallel β-folding
Stack structure, belong to orthorhombic system, peptide chain arranged regular, hydrogen bond and intermolecular gravitation make adjacent chain is intersegmental to be tightly combined, tension
It is strong to stretch ability, and is insoluble in water, it is strong to the resistance of acid, alkali, salt, enzyme and heat.In addition, recent years are found that one kind is new again
Fibroin crystal habit, i.e. the type of fibroin III, its crystal structure is similar with polyglycine II, belongs to hexagonal crystal system.
Silk obtained regenerated silk fibroin after degumming, dissolving, purification have nontoxic, non-stimulated, biological degradability,
Biocompatibility, good engineering properties, are easily processed into various forms, as silk protein films, gel, fiber, three-dimensional rack,
Sponge etc., it is a kind of important natural function material, available for fields such as biology, medical science, photoelectric materials, is carried as medicament slow release
Body, tissue engineering bracket, operation suture thread, artificial skin, artificial tendon, cell culture vector, wound dressing, electrically conducting transparent are thin
Film, sorbing material etc.（Silk, 2017,03:6-12；Biomedical engineering magazine, 2015,06:1364-1368；Sericulture section
Learn, 2016,02:341-345）.
For a long time, cellulose is always weaving, the key industry raw material of papermaking, with its recyclability, biodegradable
Property and cost advantage are increasingly subject to the attention of people, in medicine control, release tech, immobilization technology, biology sensor, membrane material
Material, performance chemicalses and additive etc. show good development prospect.Reduction and oil, natural gas due to arable land etc.
The increasingly depleted of fossil resource, the yield of synthetic fibers will be restricted more and more.And a kind of green of cellulose conduct,
Environmentally friendly, reproducible resource, obtain a unprecedented opportunity to develop.
Salix monogolica is the desert plant that a kind of only a few can be grown in salt-soda soil.Its sprout is yellow, in leaf is linear or line
Shape lanceolar, branch, which is grown thickly, is not afraid of husky pressure, and well developed root system, rudiment power is strong, is desert-control tree, be mainly distributed on the Inner Mongol,
The ground such as Hebei, Shanxi, Shaanxi, Gansu, Qinghai, Sichuan.Salix monogolica is one of the first choice of " three Norths shelter-forest ", is not only acted as windproof solid
Effect that is husky, conserving water and soil, improving the ecosystem, maintaining ecological balance etc. that also there is unique function.
Salix monogolica in addition to small part is used for pulping and paper-making, fiberboard and composite plate, burn or lose as yule logs by the overwhelming majority
Abandon, cause the huge wasting of resources.The main chemical compositions of salix monogolica mainly have cellulose, hemicellulose, lignin and ash content, fine
The content of element is tieed up in more than 60-70%, is natural reproducible biomass resource, rationally will produce huge warp using salix monogolica resource
Benefit of helping and ecological benefits.At present, most research all concentrates on the cellulose how extracted in salix monogolica.Beijing Forestry University
Department of chemistry engineering Jiang builds new et al. the influence that have studied steam blasting pretreatment to salix monogolica composition and fibre structure performance（Modernization
Work, 2008,28 (2)）.Agricultural University of the Inner Mongol's material science and School of Art and Design Zhang Bin et al. are using salix cellulose as original
Material, have studied the technique that supercritical ultrasonics technology prepares microfibril（Paper and papermaking, 2014,33 (3)）.Agricultural University of the Inner Mongol's material science
With refined et al. main chemical compositions cellulose, the hemicelluloses that salix monogolica material has been isolated using chemical reagent of School of Art and Design Li Ya
Element（Agricultural University of the Inner Mongol's journal, 2014,35 (1)）.Industry light industry textile industry institute of Qiqihar University is permitted phoenix et al. and utilizes peroxidating
Hydrogen method separates salix monogolica and the cellulose in caragana microphylla mixed material（Chemistry of forest product and industry, 2006,26 (2)）.Zhengzhou University's chemical industry
Salix cellulose is extracted with energy institute Huang star et al. use acid catalysis Ethanol Method（Jiangsu's agriculture science, 2014,42 (3)）.
And the document that salix monogolica based nano composite material is prepared using the salix cellulose of extraction as raw material is less.Such as the Inner Mongol
Agriculture university Li Ya is refined to report salix cellulose/composite titania material（Li Ya is refined, and salix celluloses/titanium dioxide is multiple
The preparation of condensation material and performance study [D] Agricultural University of the Inner Mongol, 2015）.Chinese patent CN201410701957.9 is disclosed
A kind of salix monogolica regenerated celulose fibre, Chinese patent CN201410544845.7 disclose a kind of nanometer silver antimicrobial salix monogolica again
Raw cellulose fibre, Chinese patent CN201410544055.9 disclose a kind of feature salix monogolica regenerated celulose fibre and its system
Preparation Method, a kind of graphene blending salix monogolica regenerated celulose fibres of Chinese patent CN201410544166.X and preparation method thereof.
2004, Univ Manchester UK physicist An Deliehaimu and Constantine's Nuo Woxiao loves, utilize
The method for tearing adhesive tape, successfully isolates the graphene of individual layer atomic arrangement from graphite, therefore two people also obtain 2010
The Nobel Prize in physics in year（Science,2004,306( 5696):666-669）.Graphene is by carbon atom with sp2Hydridization rail
Road forms hexangle type honeycomb lattice, and its construction unit is carbon hexatomic ring, and it is a kind of two-dimentional material of only single layer of carbon atom thickness
Material.Graphene is the basic system unit for forming carbon-based material.It can be wrapped to form zero dimension Fullerenes, be rolled into one-dimensional
Carbon nanotube, layer upon layer is into three-dimensional graphite.From graphene find that day, graphene just into
For the focus and focus of research, in ultracapacitor, transparency electrode, desalinization, light emitting diode, sensor, hydrogen storage, the sun
The fields such as energy battery, catalyst carrier, composite, biologic bracket material, bio-imaging, drug delivery, weaving, printing and dyeing have extensively
General application（Novel charcoal material, 2014,05:329-356, Chinese invention patent 201410565512.2）.
Graphene composite material is research direction important in graphene application field（Chemical Engineer, 2015,01:34-
38+46）.Existing graphene composite material is by graphene oxide and another material mostly（Inorganic material, polymeric material
Material etc.）Uniformly it is mixed in solvent, finished product is then obtained by the methods of spin processes, vacuum filtration, spin coating.But due to graphene
The problem of certain be present in the π-π stackings effect easily aggregation of itself, its dispersiveness in a solvent（Chemical progress, 2016,05:
647-656）, the preparation of follow-up composite and the final performance of product can be influenceed.
The content of the invention
In view of the above problems, the present invention provides silk fibre composite of a kind of graphene oxide parcel and preparation method thereof.
（1）1-100g/L dopamine Tris-HCl buffer solutions are prepared, regulation pH value is to 8.5, at room temperature by salix monogolica fiber
Element is immersed in 24h in above-mentioned buffer solution, bath raio 1:50, after deionized water is cleaned repeatedly, obtain poly-dopamine modified lithium salix monogolica fiber
Element；（2）Silk-fibroin is dissolved in deionized water, is configured to the 1g/L-100g/L aqueous solution, by 1g/L- under conditions of 50-80 DEG C
The 100g/L trivalent iron salt aqueous solution is slowly dropped into silk protein aqueous solution, is stirred, wherein the silk-fibroin and trivalent
The mass ratio of molysite is 1:1-10:1, calcium chloride solution of the concentration as 1-5wt% is added dropwise using 30 drops/min speed, adjusted
PH value is to 10-12, and after 60 DEG C are at the uniform velocity stirred 1h, the poly-dopamine modified lithium salix cellulose that is slowly added in step 1, ultrasound is mixed
After closing uniformly, pour into mould, be put into 1min in liquid nitrogen, pre-freeze 6h in -20 DEG C of refrigerators is placed in after taking-up, -80 DEG C of Thermo surpass
6h is freezed in low temperature refrigerator, 48h in freeze dryer is then placed in and obtains magnetic porous composite material；（3）Configuration concentration 1-100g/
L graphene oxide water solution, ultrasonic 1h, the magnetic porous composite material in step 2 is then immersed in graphene oxide water
1-12h in solution, bath raio 1:50, cleaned repeatedly with ethanol and deionized water after taking-up, graphene oxide is obtained after vacuum drying
The composite of parcel.
Preferably, the silk-fibroin is that silk is made after degumming, dissolving, dialysis, purification；
Preferably, the trivalent iron salt is the one or more in iron chloride, ferric sulfate, ferric nitrate；
Preferably, the mass ratio of the calcium chloride and silk-fibroin is 1:50.
Preferably, the mass ratio of the modified salix cellulose and silk-fibroin is 1:1.
The extraction of salix cellulose refers to Chinese invention patent CN201410544050.6, Chinese invention patent
CN201410701957.9。
Compared with prior art, the advantage of the invention is that：
（1）Poly-dopamine is a kind of biocompatible materials with superpower Adhesion property, almost can any material surface into
Film.The forming process of poly-dopamine is simple, and reaction condition is gentle, delays as long as immersing the material in the Tris-HCl of alkalescence containing dopamine
Poly-dopamine layer can be formed in fliud flushing in material surface.Thus poly-dopamine modified lithium salix cellulose effectively increases salix monogolica fibre
Bonding between dimension element and fibroin.（2）To be modified salix cellulose and silk-fibroin as carrier, nano ferriferrous oxide is generated
Particle, and it is composite porous to obtain after crosslinking, liquid nitrogen, freeze-drying process silk-salix monogolica, final load graphite oxide
Alkene, ensure that dispersing uniformity and silk-salix monogolica porous material of the nano material in silk-salix monogolica matrix Stability Analysis of Structures and
Mechanical strength, silk-salix monogolica composite after calcium ion crosslinking have density is low, intensity is big, high temperature resistant, specific surface area are big,
The advantages that adsorption capacity is strong.（3）Composite has certain magnetic, it is possible to achieve effective to recycle.
Embodiment
The invention will be further elucidated with reference to specific embodiments.
Embodiment 1：
（1）10g/L dopamine Tris-HCl buffer solutions are prepared, salix cellulose is immersed in by regulation pH value at room temperature to 8.5
24h in above-mentioned buffer solution, bath raio 1:50, after deionized water is cleaned repeatedly, obtain poly-dopamine modified lithium salix cellulose；（2）Will
Silk-fibroin is dissolved in deionized water, is configured to the 10g/L aqueous solution, is delayed 10g/L ferric chloride in aqueous solution under conditions of 50 DEG C
Slowly it is added dropwise in silk protein aqueous solution, stirs, wherein the mass ratio of the silk-fibroin and iron chloride is 1:1, with 30 drop/
The calcium chloride solution that concentration is 1wt% is added dropwise in min speed, and the mass ratio of calcium chloride and silk-fibroin is 1:50, adjust pH value
After at the uniform velocity 1h being stirred to 10,60 DEG C, the poly-dopamine modified lithium salix cellulose that is slowly added in step 1, modified salix cellulose
Mass ratio with silk-fibroin is 1:1, after ultrasonic mixing is uniform, pour into mould, be put into 1min in liquid nitrogen, -20 are placed in after taking-up
Pre-freeze 6h in DEG C refrigerator, 6h is freezed in -80 DEG C of Thermo ultra low temperature freezers, being then placed in 48h in freeze dryer, to obtain magnetic more
Hole composite material；（3）Configuration concentration 10g/L graphene oxide water solution, ultrasonic 1h then will be magnetic porous in step 2
Composite is immersed in 1h in graphene oxide water solution, bath raio 1:50, cleaned repeatedly with ethanol and deionized water after taking-up, very
Sky obtains the silk fibre composite of graphene oxide parcel after drying.
Embodiment 2：
（1）30g/L dopamine Tris-HCl buffer solutions are prepared, salix cellulose is immersed in by regulation pH value at room temperature to 8.5
24h in above-mentioned buffer solution, bath raio 1:50, after deionized water is cleaned repeatedly, obtain poly-dopamine modified lithium salix cellulose；（2）Will
Silk-fibroin is dissolved in deionized water, is configured to the 20g/L aqueous solution, is delayed 20g/L ferric sulfate aqueous solution under conditions of 80 DEG C
Slowly it is added dropwise in silk protein aqueous solution, stirs, wherein the mass ratio of the silk-fibroin and ferric sulfate is 3:1, with 30 drop/
The calcium chloride solution that concentration is 2wt% is added dropwise in min speed, and the mass ratio of calcium chloride and silk-fibroin is 1:50, adjust pH value
After at the uniform velocity 1h being stirred to 11,60 DEG C, the poly-dopamine modified lithium salix cellulose that is slowly added in step 1, modified salix cellulose
Mass ratio with silk-fibroin is 1:1, after ultrasonic mixing is uniform, pour into mould, be put into 1min in liquid nitrogen, -20 are placed in after taking-up
Pre-freeze 6h in DEG C refrigerator, 6h is freezed in -80 DEG C of Thermo ultra low temperature freezers, being then placed in 48h in freeze dryer, to obtain magnetic more
Hole composite material；（3）Configuration concentration 50g/L graphene oxide water solution, ultrasonic 1h then will be magnetic porous in step 2
Composite is immersed in 6h in graphene oxide water solution, bath raio 1:50, cleaned repeatedly with ethanol and deionized water after taking-up, very
Sky obtains the silk fibre composite of graphene oxide parcel after drying.
Embodiment 3：
（1）50g/L dopamine Tris-HCl buffer solutions are prepared, salix cellulose is immersed in by regulation pH value at room temperature to 8.5
24h in above-mentioned buffer solution, bath raio 1:50, after deionized water is cleaned repeatedly, obtain poly-dopamine modified lithium salix cellulose；（2）Will
Silk-fibroin is dissolved in deionized water, is configured to the 50g/L aqueous solution, is delayed 50g/L iron nitrate aqueous solution under conditions of 60 DEG C
Slowly it is added dropwise in silk protein aqueous solution, stirs, wherein the mass ratio of the silk-fibroin and ferric nitrate is 2:1, with 30 drop/
The calcium chloride solution that concentration is 5wt% is added dropwise in min speed, and the mass ratio of calcium chloride and silk-fibroin is 1:50, adjust pH value
After at the uniform velocity 1h being stirred to 12,60 DEG C, the poly-dopamine modified lithium salix cellulose that is slowly added in step 1, modified salix cellulose
Mass ratio with silk-fibroin is 1:1, after ultrasonic mixing is uniform, pour into mould, be put into 1min in liquid nitrogen, -20 are placed in after taking-up
Pre-freeze 6h in DEG C refrigerator, 6h is freezed in -80 DEG C of Thermo ultra low temperature freezers, being then placed in 48h in freeze dryer, to obtain magnetic more
Hole composite material；（3）Configuration concentration 80g/L graphene oxide water solution, ultrasonic 1h then will be magnetic porous in step 2
Composite is immersed in 12h in graphene oxide water solution, bath raio 1:50, cleaned repeatedly with ethanol and deionized water after taking-up,
The silk fibre composite of graphene oxide parcel is obtained after vacuum drying.
Obviously, the above embodiment of the present invention is only intended to clearly illustrate example of the present invention, and is not pair
The restriction of embodiments of the present invention.For those of ordinary skill in the field, may be used also on the basis of the above description
To make other changes in different forms.Here all embodiments can not be exhaustive.It is every to belong to this hair
Row of the obvious changes or variations that bright technical scheme is amplified out still in protection scope of the present invention.
Claims (6)
- A kind of 1. preparation method of the silk fibre composite of graphene oxide parcel, it is characterised in that：Step 1：1-100g/L dopamine Tris-HCl buffer solutions are prepared, regulation pH value is to 8.5, at room temperature by salix monogolica fiber Element is immersed in 24h in above-mentioned buffer solution, bath raio 1:50, after deionized water is cleaned repeatedly, obtain poly-dopamine modified lithium salix monogolica fiber Element；Step 2：Silk-fibroin is dissolved in deionized water, is configured to the 1g/L-100g/L aqueous solution, will under conditions of 50-80 DEG C The 1g/L-100g/L trivalent iron salt aqueous solution is slowly dropped into silk protein aqueous solution, is stirred, wherein the silk-fibroin and The mass ratio of trivalent iron salt is 1:1-10:1, calcium chloride solution of the concentration as 1-5wt% is added dropwise using 30 drops/min speed, PH value is adjusted to 10-12, after 60 DEG C are at the uniform velocity stirred 1h, the poly-dopamine modified lithium salix cellulose that is slowly added in step 1 surpasses After sound is well mixed, pours into mould, be put into 1min in liquid nitrogen, be placed in pre-freeze 6h in -20 DEG C of refrigerators after taking-up, -80 DEG C 6h is freezed in Thermo ultra low temperature freezers, 48h in freeze dryer is then placed in and obtains magnetic porous composite material；Step 3：Configuration concentration 1-100g/L graphene oxide water solution, ultrasonic 1h then will be magnetic porous in step 2 Composite is immersed in 1-12h in graphene oxide water solution, bath raio 1:50, it is repeatedly clear with ethanol and deionized water after taking-up Wash, the silk fibre composite of graphene oxide parcel is obtained after vacuum drying.
- 2. a kind of preparation method of the silk fibre composite of graphene oxide parcel according to claim 1, its feature exist In the silk-fibroin is that silk is made after degumming, dissolving, dialysis, purification.
- 3. a kind of preparation method of the silk fibre composite of graphene oxide parcel according to claim 1, its feature exist In the trivalent iron salt is the one or more in iron chloride, ferric sulfate, ferric nitrate.
- 4. a kind of preparation method of the silk fibre composite of graphene oxide parcel according to claim 1, its feature exist In the mass ratio of the calcium chloride and silk-fibroin is 1:50.
- 5. a kind of preparation method of the silk fibre composite of graphene oxide parcel according to claim 1, its feature exist In the mass ratio of the modified salix cellulose and silk-fibroin is 1:1.
- 6. the silk fibre composite that a kind of graphene oxide obtained by claim 1 preparation method wraps up.
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| CN106400205A (en) * | 2016-11-21 | 2017-02-15 | 江南大学 | Preparation method of hollow magnetic iron oxide nanofiber |
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| CN101358382A (en) * | 2008-08-26 | 2009-02-04 | 东华大学 | Antibacterial nano fiber material and preparation method thereof |
| CN102758356A (en) * | 2012-07-19 | 2012-10-31 | 陕西科技大学 | Process for enhancing hygiene performance of superfine-fiber synthetic leather |
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Application publication date: 20180105 |