CN104264259A - Graphene and salix psammophila regenerated cellulose blended fiber and preparation method thereof - Google Patents
Graphene and salix psammophila regenerated cellulose blended fiber and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a graphene and salix psammophila regenerated cellulose blended fiber and a preparation method thereof. The preparation method comprises steps as follows: peeling, crushing, sieving, drying and cooling salix psammophila to prepare salix psammophila wood meal; extracting salix psammophila cellulose with an ethanol-acid mixed liquid; performing technological treatment such as cooking, bleaching and the like on the salix psammophila cellulose to obtain salix psammophila pulp; performing filtration and reduced pressure defoaming on graphene oxide and the salix psammophila cellulose to obtain an evenly mixed spinning solution; performing coagulating bath spinning, drawing forming, reining and drying on the spinning solution; finally, performing reduction to obtain the graphene and salix psammophila regenerated cellulose blended fiber. According to the method, the graphene oxide and the salix psammophila regenerated cellulose are taken as raw materials, and the functional regenerated cellulose fiber with the anti-static property, the antibacterial property, the high strength and the good wearability is prepared with efficient blending, wet spinning and after-treatment reduction technologies.
Description
Technical field
The present invention relates to blended salix monogolica regenerated celulose fibre of a kind of Graphene and preparation method thereof, belong to natural polymer and field of textiles.
Background technology
For a long time, cellulose is the key industry raw material of weaving, papermaking always, day by day be subject to people's attention with its recyclability, biodegradability and cost advantage, in medicine control, release tech, immobilization technology, biology sensor, membrane material, performance chemicals and additive etc., demonstrate good development prospect.Due to the minimizing in arable land and the day by day exhausted of the fossil resource such as oil, natural gas, the output of natural fabric, synthetic fiber will be subject to increasing restriction.And regenerated cellulose is as a kind of green, environmental protection, reproducible resource, obtain a unprecedented opportunity to develop.
Salix monogolica is the desert plant that a kind of only a few can grow in salt-soda soil.Its sprout is yellow, the linear or wire lanceolar in leaf, and branch is grown thickly and is not afraid of husky pressure, well developed root system, and rudiment power is strong, is desert-control tree, is mainly distributed in the ground such as the Inner Mongol, Hebei, Shanxi, Shaanxi, Gansu, Qinghai, Sichuan.Salix monogolica is one of the first-selection of " three Norths shelter-forest ", not only plays the effect of checking winds and fixing drifting sand, conserving water and soil, and is improving the function also in the ecosystem, the maintenance ecological balance etc. with uniqueness.
Salix monogolica is except small part is used for pulping and paper-making, fiberboard and composite plate, and the overwhelming majority is as yule logs burning or abandon, and causes the huge wasting of resources.The main chemical compositions of salix monogolica mainly contains cellulose, hemicellulose, lignin and ash content, and cellulosic content, at more than 60-70%, is natural reproducible biomass resource, and Appropriate application salix monogolica resource is by the huge economic benefit of generation 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 and new waits people to have studied the impact (modern chemical industry, 2008,28 (2)) of steam blasting preliminary treatment on salix monogolica composition and fibre structure performance.The people such as Agricultural University of the Inner Mongol's material science and School of Art and Design Zhang Bin for raw material, have studied the technique (paper and papermaking, 2014,33 (3)) that supercritical ultrasonics technology prepares microfibril with salix monogolica cellulose.Main chemical compositions cellulose, the hemicellulose (Agricultural University of the Inner Mongol's journal, 2014,35 (1)) of Agricultural University of the Inner Mongol's material science and people utilized chemical reagent the to isolate salix monogolica material such as School of Art and Design Li Ya is refined.The people such as industry light industry textile industry institute of Qiqihar University Xu Feng utilize the cellulose (chemistry of forest product and industry, 2006,26 (2)) in hydrogen peroxide method separation salix monogolica and caragana microphylla mixed material.The people such as Zhengzhou University's chemical industry and the yellow star of energy institute adopt acid catalysis Ethanol Method to extract salix monogolica cellulose (Jiangsu's agriculture science, 2014,42 (3)).But there are no document by the salix monogolica cellulose that extracts for the preparation of salix monogolica regenerated cellulose.
2004, Univ Manchester UK physicist An Deliehaimu and Constantine Nuo Woxiaoluofu, utilize the method for tearing adhesive tape, from graphite, successfully isolate the Graphene of individual layer atomic arrangement, therefore two people also obtain the Nobel Prize in physics (Science of 2010,2004,306 (5696): 666-669).Graphene by carbon atom with sp
2hybridized orbit composition hexangle type honeycomb lattice, its construction unit is carbon hexatomic ring, and it is a kind of two-dimensional material only having monolayer carbon atomic thickness.Graphene is the basic system unit forming carbon-based material.It can be wrapped to form zero dimension Fullerenes, is rolled into one dimension carbon nanotube, is piled into three-dimensional graphite layer by layer.From that day that Graphene finds, Graphene has just become focus and the focus of research, is widely used in fields such as ultracapacitor, transparency electrode, desalinization, light emitting diode, sensor, Chu Qing, solar cell, catalyst carrier, composite, biologic bracket material, bio-imaging, drug delivery, weaving, printing and dyeing.
Graphene has excellent machinery, electricity, thermal property (printing and dyeing, 2014 (5): 49-52).Graphene is material the thinnest in the world, and it only has the thickness of individual layer atom, is about 0.335nm.Graphene is almost completely transparent, and only absorb the light of 2.3%, light transmittance is up to 97.7%.Resistivity 10
-6Ω/cm, than copper or silver lower, be the material that at present resistivity is minimum in the world.Graphene has great specific area, and its theoretical value is up to 2630m
2/ g.Thermal conductivity factor is up to 5300W/mK, and under normal temperature, electron mobility is more than 15000cm
2/ Vs, than CNT and monocrystalline silicon high.Young's modulus is 1.1TPa, and fracture strength is up to 130GPa.Recent research shows that Graphene has good anti-microbial property equally.
But Graphene, due to intermolecular extremely strong active force, is insoluble in water and organic solvent.Graphene oxide (GO) is the growth of Graphene, substantially identical with the structure of Graphene, but graphene oxide basal plane and edge contain the functional groups such as hydroxyl-OH, carboxyl-COOH, carbonyl C=O.The water-soluble of graphene oxide (GO) is better than Graphene.GO contains active group, can carry out covalent reaction with other chemical group.
In view of Graphene gathers around so many high-quality characteristic, if with graphene oxide and regenerated cellulose for raw material, can be prepared by efficiently blended, wet spinning and post processing reduction technique have that antistatic property is good, the functional regenerated cellulose fibre of anti-microbial property, high strength and good wearability.
Summary of the invention
The present invention is directed to above-mentioned deficiency, blended salix monogolica regenerated celulose fibre of a kind of Graphene and preparation method thereof is provided.
The present invention is achieved by following technical proposals:
(1) salix monogolica wood powder is prepared: removed the peel by salix monogolica, pulverize, cross 50-100 mesh sieve, 80-100 DEG C of oven dry, cooling, puts into drier for subsequent use;
(2) salix monogolica fiber is prepared: by the salix monogolica wood powder in step one, add in autoclave, add absolute ethyl alcohol-sour mixed liquor, solid-to-liquid ratio 1:5-1:20, after being heated to 100-160 DEG C, stir 1-5h, cooling, filters, with absolute ethanol washing 2-5 time, repeatedly rinse well with deionized water again, dry;
(3) prepare salix monogolica pulp: the NaOH boiling adopting 5-15%wt, bath raio is 1:5-1:10, boiling temperature 200-250 DEG C, time 3-5h, then the hydrogen peroxide bleaching adopting 20-25%wt, bleaching temperature 80-100 DEG C, bleaching time 1-2h;
(4) the blended salix monogolica spinning solution of graphene oxide is prepared: according to the volume ratio of 1:10-1:100, by ultrasonic for the graphene oxide solution of 0.01-0.5%wt 1-24h, slowly be added drop-wise to 80 DEG C of stirring 1-10h in the salix monogolica cellulose solution of 10-20%wt, obtain the spinning solution mixed after filtration with vacuum deaerator;
(5) the blended salix monogolica regenerated celulose fibre of graphene oxide is prepared: by spinning solution through coagulating bath spinning, draw forming, then refining, oven dry;
(6) the blended salix monogolica regenerated celulose fibre of redox graphene: the reductant solution choosing 2-20%wt, the blended salix monogolica regenerated celulose fibre of graphene oxide is taken in the ratio of bath raio 1:10-1:20, under 50-80 DEG C of condition, blended for graphene oxide salix monogolica regenerated celulose fibre is placed on reductase 12-24h in reductant solution, and washing can obtain the blended salix monogolica regenerated celulose fibre of Graphene after drying.
Preferably, the acid in described step (2) is one or more in sulfuric acid, nitric acid, hydrochloric acid, acetic acid, and addition is 3-5%wt.
Preferably, the coagulation bath temperature in described step (5) is 40-60 DEG C, sulfur acid 100-130g/l, zinc sulfate 15-20g/l, sodium sulphate 320-360g/l in coagulating bath, drafting multiple 1.8-2.0.
Preferably, the reductant in described step (6) is one or more in hydrazine hydrate, sodium borohydride, hydroiodic acid, natrium citricum, Tea Polyphenols.
Compared with prior art, the invention has the advantages that: the present invention with graphene oxide and salix monogolica regenerated cellulose for raw material, the blended salix monogolica regenerated celulose fibre of Graphene with high strength, antistatic property, anti-microbial property is prepared by efficiently blended, wet spinning and post processing reduction technique, improve the utilization rate of salix monogolica resource, the field such as clothes and fabrics for industrial use can be widely used in, produce huge economic benefit and ecological benefits.
Detailed description of the invention
Below in conjunction with detailed description of the invention, set forth the present invention further.
Embodiment 1:
(1) salix monogolica wood powder is prepared: removed the peel by salix monogolica, pulverize, cross 100 mesh sieves, 80 DEG C of oven dry, cooling, puts into drier for subsequent use;
(2) salix monogolica fiber is prepared: by the salix monogolica wood powder in step (1), add in autoclave, add absolute ethyl alcohol-nitric acid mixed liquor, wherein nitric acid addition is 3%wt, solid-to-liquid ratio 1:10, after being heated to 120 DEG C, stir 3h, cooling, filter, with absolute ethanol washing 5 times, more repeatedly rinse well with deionized water, dry;
(3) prepare salix monogolica pulp: the NaOH boiling adopting 10%wt, bath raio is 1:10, boiling temperature 200 DEG C, time 3h, then the hydrogen peroxide bleaching adopting 20%wt, bleaching temperature 100 DEG C, bleaching time 2h;
(4) the blended salix monogolica spinning solution of graphene oxide is prepared: according to the volume ratio of 1:10, by the graphene oxide solution ultrasonic vibration 24h of 0.5%wt, slowly be added drop-wise to 80 DEG C of stirring 10h in the salix monogolica cellulose solution of 10%wt, obtain the spinning solution mixed after filtration with vacuum deaerator;
(5) the blended salix monogolica regenerated celulose fibre of graphene oxide is prepared: by spinning solution through coagulating bath spinning, draw forming, then refining, oven dry, wherein coagulation bath temperature is 60 DEG C, sulfur acid 100g/l, zinc sulfate 15g/l, sodium sulphate 320g/l in coagulating bath, drafting multiple 2.0.
(6) the blended salix monogolica regenerated celulose fibre of redox graphene: the hydrazine hydrate choosing 5%wt, the blended salix monogolica regenerated celulose fibre of graphene oxide is taken in the ratio of bath raio 1:10, under 50 DEG C of conditions, be placed in hydrazine hydrate by blended for graphene oxide salix monogolica regenerated celulose fibre and reduce 12h, washing can obtain the blended salix monogolica regenerated celulose fibre of Graphene after drying.
According to the blended salix monogolica regenerated celulose fibre of Graphene prepared by embodiment 1, dry strong 2.31cN/dtex, reach 90.3% to the bacteriostasis rate of staphylococcus aureus, Escherichia coli bacteriostasis rate reaches 85%, surface specific resistance=4.5 × 10
6Ω/m
2.Wherein bacteriostasis rate is tested according to shake flasks method in Unite States Standard ASTM E2149 and GB FZ/T 73023-2006.
Embodiment 2:
(1) salix monogolica wood powder is prepared: removed the peel by salix monogolica, pulverize, cross 80 mesh sieves, 90 DEG C of oven dry, cooling, puts into drier for subsequent use;
(2) salix monogolica fiber is prepared: by the salix monogolica wood powder in step (1), add in autoclave, add absolute ethyl alcohol-sulfuric acid mixture liquid, wherein sulfuric acid addition is 4%wt, solid-to-liquid ratio 1:5, after being heated to 120 DEG C, stir 2h, cooling, filter, with absolute ethanol washing 3 times, more repeatedly rinse well with deionized water, dry;
(3) prepare salix monogolica pulp: the NaOH boiling adopting 5%wt, bath raio is 1:5, boiling temperature 250 DEG C, time 4h, then the hydrogen peroxide bleaching adopting 25%wt, bleaching temperature 80 DEG C, bleaching time 1h;
(4) the blended salix monogolica spinning solution of graphene oxide is prepared: according to the volume ratio of 1:50, by the graphene oxide solution ultrasonic vibration 12h of 0.1%wt, slowly be added drop-wise to 80 DEG C of stirring 5h in the salix monogolica cellulose solution of 15%wt, obtain the spinning solution mixed after filtration with vacuum deaerator;
(5) the blended salix monogolica regenerated celulose fibre of graphene oxide is prepared: by spinning solution through coagulating bath spinning, draw forming, then refining, oven dry, wherein coagulation bath temperature is 40 DEG C, sulfur acid 120g/l, zinc sulfate 20g/l, sodium sulphate 360g/l in coagulating bath, drafting multiple 1.8.
(6) the blended salix monogolica regenerated celulose fibre of redox graphene: the sodium borohydride choosing 5%wt, the blended salix monogolica regenerated celulose fibre of graphene oxide is taken in the ratio of bath raio 1:10-1:20, under 60 DEG C of conditions, be placed in sodium borohydride by blended for graphene oxide salix monogolica regenerated celulose fibre and reduce 8h, washing can obtain the blended salix monogolica regenerated celulose fibre of Graphene after drying.
Embodiment 3:
(1) salix monogolica wood powder is prepared: removed the peel by salix monogolica, pulverize, cross 60 mesh sieves, 80 DEG C of oven dry, cooling, puts into drier for subsequent use;
(2) salix monogolica fiber is prepared: by the salix monogolica wood powder in step (1), add in autoclave, add absolute ethyl alcohol-hydrochloric acid mixed solution, solid-to-liquid ratio 1:15, after being heated to 140 DEG C, stir 3h, cooling, filter, with absolute ethanol washing 2 times, more repeatedly rinse well with deionized water, dry;
(3) prepare salix monogolica pulp: the NaOH boiling adopting 15%wt, bath raio is 1:10, boiling temperature 220 DEG C, time 3h, then the hydrogen peroxide bleaching adopting 20%wt, bleaching temperature 80 DEG C, bleaching time 2h;
(4) the blended salix monogolica spinning solution of graphene oxide is prepared: according to the volume ratio of 1:100, by the graphene oxide solution ultrasonic vibration 10h of 0.08%wt, slowly be added drop-wise to 80 DEG C of stirring 8h in the salix monogolica cellulose solution of 20%wt, obtain the spinning solution mixed after filtration with vacuum deaerator;
(5) the blended salix monogolica regenerated celulose fibre of graphene oxide is prepared: by spinning solution through coagulating bath spinning, draw forming, then refining, oven dry, wherein coagulation bath temperature is 50 DEG C, sulfur acid 110g/l, zinc sulfate 15g/l, sodium sulphate 350g/l in coagulating bath, drafting multiple 1.9.
(6) the blended salix monogolica regenerated celulose fibre of redox graphene: the natrium citricum choosing 12%wt, the blended salix monogolica regenerated celulose fibre of graphene oxide is taken in the ratio of bath raio 1:15, under 70 DEG C of conditions, be placed in natrium citricum by blended for graphene oxide salix monogolica regenerated celulose fibre and reduce 18h, washing can obtain the blended salix monogolica regenerated celulose fibre of Graphene after drying.
Obviously, the above embodiment of the present invention is only for example of the present invention is clearly described, and is not the restriction to embodiments of the present invention.For those of ordinary skill in the field, can also make other changes in different forms on the basis of the above description.Here cannot give exhaustive to all embodiments.Every belong to technical scheme of the present invention the apparent change of amplifying out or variation be still in the row of protection scope of the present invention.
Claims (5)
1. blended salix monogolica regenerated celulose fibre of Graphene and preparation method thereof, is characterized in that:
Step one, preparation salix monogolica wood powder: removed the peel by salix monogolica, pulverize, cross 50-100 mesh sieve, 80-100 DEG C of oven dry, cooling, puts into drier for subsequent use;
Step 2, preparation salix monogolica fiber: by the salix monogolica wood powder in step one, add in autoclave, add absolute ethyl alcohol-sour mixed liquor, solid-to-liquid ratio 1:5-1:20, after being heated to 100-160 DEG C, stir 1-5h, cooling, filter, with absolute ethanol washing 2-5 time, more repeatedly rinse well with deionized water, dry;
Step 3, preparation salix monogolica pulp: the NaOH boiling adopting 5-15%wt, bath raio is 1:5-1:10, boiling temperature 200-250 DEG C, time 3-5h, then the hydrogen peroxide bleaching adopting 20-25%wt, bleaching temperature 80-100 DEG C, bleaching time 1-2h;
Step 4, prepare graphene oxide blended salix monogolica spinning solution: according to certain volume ratio, by ultrasonic for the graphene oxide solution of 0.01-0.5%wt 1-24h, slowly be added drop-wise to 80 DEG C of stirring 1-10h in the salix monogolica cellulose solution of 10-20%wt, obtain the spinning solution mixed after filtration with vacuum deaerator;
Step 5, prepares the blended salix monogolica regenerated celulose fibre of graphene oxide: by spinning solution through coagulating bath spinning, draw forming, then refining, oven dry;
Step 6, the blended salix monogolica regenerated celulose fibre of redox graphene: the reductant solution choosing 2-20%wt, the blended salix monogolica regenerated celulose fibre of graphene oxide is taken in the ratio of bath raio 1:10-1:20, under 50-80 DEG C of condition, blended for graphene oxide salix monogolica regenerated celulose fibre is placed on reductase 12-24h in reductant solution, and washing can obtain the blended salix monogolica regenerated celulose fibre of Graphene after drying.
2. blended salix monogolica regenerated celulose fibre of a kind of Graphene according to claim 1 and preparation method thereof, is characterized in that, the acid described in step 2 is one or more in sulfuric acid, nitric acid, hydrochloric acid, acetic acid, and addition is 3-5%wt.
3. blended salix monogolica regenerated celulose fibre of a kind of Graphene according to claim 1 and preparation method thereof, is characterized in that, the volume ratio described in step 4 is 1:10-1:100.
4. blended salix monogolica regenerated celulose fibre of a kind of Graphene according to claim 1 and preparation method thereof, it is characterized in that, coagulation bath temperature in step 5 is 40-60 DEG C, sulfur acid 100-130g/l, zinc sulfate 15-20g/l, sodium sulphate 320-360g/l in coagulating bath, drafting multiple 1.8-2.0.
5. blended salix monogolica regenerated celulose fibre of a kind of Graphene according to claim 1 and preparation method thereof, is characterized in that, the reductant in step 6 is one or more in hydrazine hydrate, sodium borohydride, hydroiodic acid, natrium citricum, Tea Polyphenols.
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| CN107556518A (en) * | 2017-09-17 | 2018-01-09 | 钱景 | Graphene oxide salix monogolica konjaku cyclodextrin composite and preparation method |
| CN107556761A (en) * | 2017-09-17 | 2018-01-09 | 钱景 | A kind of graphene/silk/salix monogolica nano composite material and preparation method thereof |
| CN107619500A (en) * | 2017-09-17 | 2018-01-23 | 钱景 | A kind of graphene salix monogolica konjaku magnetic composite and preparation method thereof |
| CN108277545A (en) * | 2018-01-19 | 2018-07-13 | 杭州高烯科技有限公司 | A kind of preparation method of multifunction regenerated cellulose composite fibre |
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Application publication date: 20150107 |