CN107630349A - Multifunctional cellulose fiber based on graphene oxide/nano zine oxide - Google Patents
Multifunctional cellulose fiber based on graphene oxide/nano zine oxide Download PDFInfo
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Abstract
The invention discloses a kind of Multifunctional cellulose fiber based on graphene oxide/nano zine oxide and preparation method thereof, cationized cellulose fiber is immersed in anionic burnett's solution system and cationic burnett's solution system successively and carries out self assembly, one layer of graphene oxide finally is wrapped up in cellulose fibre outermost layer, obtains the Multifunctional cellulose fiber based on graphene oxide/nano zine oxide.Nano zine oxide imparts the excellent antibacterial of cellulose fibre, uvioresistant, crease-resistant, yellowing-resistant and performance, the graphene oxide such as washable and wraps up the biological safety for effectively increasing inorganic nano material by electrostatic attraction LBL self-assembly strong bonded.Electrostatic layer-by-layer, nano zine oxide and graphene oxide are applied to field of textiles by the present invention, contribute to the present situation for overcoming textile industry single varieties, with low content of technology, added value of product not high, it is significant for the transition and upgrade and sustainable development of realizing textile industry.
Description
Technical field
The present invention relates to a kind of Multifunctional cellulose fiber based on graphene oxide/nano zine oxide, belongs to field of textiles.
Background technology
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（The preparation of dissaving polymer and the function to cotton fiber
Change and be modified [D] University Of Suzhou, 2009）.
Inorganic nano material refers to that size is in 1-100nm material, relative to other nano materials, inorganic nano material
With preparing simple, the advantage such as cost is cheap, uniform particle diameter, photocatalysis, solar cell, biology, medicine, weaving, printing and dyeing,
There are extensive research and application in the fields such as wearable electronic.In the inorganic nano material of numerous types, zinc oxide accounts for
According to important position.Nano zine oxide is a kind of important photoelectric semiconductor material, has wider forbidden band wide at room temperature
Degree（3.37eV）With larger exciton bind energy.It has many excellent physical and chemical properties, such as higher chemically stable
Property, nontoxic and non-migratory, low-k, photocatalysis performance, fluorescence, piezoelectricity, absorb the ability with scatters ultraviolet
Deng, therefore nano zine oxide all has important Research Significance in many fields, and show tempting application prospect.In recent years
Nano zine oxide is used as catalyst, gas sensor, semiconductor devices, piezo-resistance, piezoelectric device, field-emitter display
It is widely used with ultraviolet light screening material etc..
In field of textiles, nano zine oxide can be used for antibacterial and deodoring materials, ultraviolet shielding material, fluorescence and catalysis material
Material etc..Zinc oxide is combined with cellulose fibre can be effectively improved cellulose fibre inherent shortcoming, expand cellulose fibre and fit
With scope, the added value of cellulose fibre is improved.By the most frequently used cellulose fibre --- exemplified by cotton fiber, use is nano oxidized
Zinc modification can assign the performances such as the excellent antibacterial of cotton fiber, uvioresistant, crease-resistant, yellowing-resistant（Hu Xiangyu are based on nano zine oxide
Super-hydrophobic uvioresistant Cotton Fabric [D] Donghua University, 2013；Zhang Ruiping, Yang Jingxin, You Ke are non-, and nano zine oxides exist
Application [J] Shanghai Textiles science and technology in functional finish of cotton fabric, 2005, (12):14-16；Wang Hao, Huang Chen, Lin Hong, Chen Yu
Nano zine oxide anti UV finishing [J] printing and dyeing of high mountain baftas, 2006, (06):1-3）.
But modification of the nano zine oxide to cellulose fibre is mainly realized by finishing method at present.Finishing method
It is main using impregnate, pad, coating or the methods of spraying by nano material arrangement to fiber, and be allowed to anchor at textile material
On a kind of method.Finishing method has that technique is simple, the advantage such as workable.But it is easy nano material in process to be present
Reunite, nano material is in fiber and fabric face skewness, the problem of nano material is low with fiber binding strength（It is hyperbranched
The preparation of polymer nano material and study on the modification [D] the University Of Suzhou to textile, 2013）.
The content of the invention
In view of the above problems, the present invention provides the Multifunctional cellulose fiber based on graphene oxide/nano zine oxide and
Its preparation method.
The technical scheme is that：
（1）Cellulose fibre is placed in the sodium hydroxide solution that mass fraction is 20%, bath raio 1:50,90 DEG C of reaction 120min,
Neutrality is washed till repeatedly with deionized water, and sodium hydroxide modified cellulose fibre is obtained after drying；Then sodium hydroxide is modified fine
Cellulose fiber is scattered in deionized water again, bath raio 1:50, add trimethylallylammonium chloride, wherein trimethyl allyl
The mass ratio of ammonium chloride and sodium hydroxide modified cellulose fibre is 1:5-1:10,60-80 DEG C of reaction 1-24h, use deionized water
Clean repeatedly, trimethylallylammonium chloride modified cellulose fibre is obtained after drying；Trimethylallylammonium chloride is modified
Cellulose fibre is scattered in deionized water again, bath raio 1:50, the polyamide-amide PAMAM for being slowly added to 1-100g/L is water-soluble
The volume ratio of liquid, the PAMAM aqueous solution and the trimethylallylammonium chloride modified cellulose fibre aqueous solution is 1:5-1:10,
75-95 DEG C of reaction 60-120min, cleaning, drying obtains cationized cellulose fiber after taking-up.（2）Prepare 1mol/L chlorination
Zinc solution, 1mol/L sodium hydrate aqueous solution, the volume of the sodium hydroxide solution and liquor zinci chloridi is then added dropwise
Than for 1:2-2:1, after ultrasonic mixing is uniform, it is slowly added to lauryl sodium sulfate, the lauryl sodium sulfate and zinc chloride
Mass ratio be 1:1-3:1, ultrasonic 2h, 160 DEG C of reaction 6-12h in reactor are moved to, cleaned repeatedly with ethanol and deionized water,
Zinc oxide nanoparticle is obtained after centrifugation, drying process.（3）PAMAM and zinc nitrate hexahydrate are configured to 1-100g/L respectively
With the 1mol/L aqueous solution, the volume ratio of PAMAM and the zinc nitrate hexahydrate aqueous solution is 1:1-5:1, it is mixed evenly
Afterwards, 200 DEG C of reaction 5h in reactor are moved to, cleaned repeatedly with ethanol and deionized water, centrifuge, zinc oxide is obtained after drying process
Nano particle.（4）Zinc oxide nanoparticle in step 2 is configured to the mass fraction 0.1-5% aqueous solution, then by step
Cationized cellulose fiber impregnation in one 30-60min, bath raio 1 in the nano zine oxide aqueous solution:10, spent after taking-up
Ionized water rinses repeatedly, drying；Then the Zinc oxide nanoparticle in step 3 is configured to the water-soluble of mass fraction 0.1-5%
Liquid, above-mentioned cellulose fibre is immersed in 30-60min in the nano zine oxide aqueous solution, bath raio 1:10, use deionized water after taking-up
Rinse, dry repeatedly, so far by one layer of nano zinc oxide to the surface of cellulose fibre, subsequent repeatedly aforesaid operations,
The number of plies of cellulose fiber surface nano zinc oxide is determined as needed.（5）Above-mentioned cellulose fibre is placed in 80 DEG C, 1-
60-600min in 20g/L graphene oxide water solution, bath raio 1:50, rinsed repeatedly with deionized water after taking-up, drying obtains
Multifunctional cellulose fiber based on graphene oxide/nano zine oxide.
Compared with prior art, the advantage of the invention is that：Nano zine oxide is firm by electrostatic attraction LBL self-assembly
With reference to imparting the excellent antibacterial of cellulose fibre, uvioresistant, crease-resistant, yellowing-resistant and the performance such as washable, graphene oxide parcel
Effectively increase the biological safety of inorganic nano material.The present invention is by electrostatic layer-by-layer, nano zine oxide and oxygen
Graphite alkene is applied to field of textiles, helps to overcome textile industry single varieties, with low content of technology, added value of product is not high
Present situation, it is significant for the transition and upgrade and sustainable development of realizing textile industry.
Embodiment
The invention will be further elucidated with reference to specific embodiments.
Embodiment 1：
（1）Cotton is placed in the sodium hydroxide solution that mass fraction is 20%, bath raio 1:50,90 DEG C reaction 120min, spend from
Sub- water is washed till neutrality repeatedly, and sodium hydroxide is obtained after drying and is modified cotton；Then sodium hydroxide modification cotton is scattered in again
In deionized water, bath raio 1:50, trimethylallylammonium chloride is added, wherein trimethylallylammonium chloride and sodium hydroxide changes
Property cotton mass ratio be 1:5,60 DEG C of reaction 1h, are cleaned, trimethyl allyl chlorination are obtained after drying repeatedly with deionized water
Ammonium is modified cotton；Trimethylallylammonium chloride modification cotton is scattered in deionized water again, bath raio 1:50, it is slowly added to
The 1g/L polyamide-amide PAMAM aqueous solution, the PAMAM aqueous solution are modified the cotton aqueous solution with trimethylallylammonium chloride
Volume ratio be 1:5,75 DEG C of reaction 60min, cleaning, drying obtains the cotton that is cationized after taking-up.（2）Prepare 1mol/L chlorine
Change zinc solution, 1mol/L sodium hydrate aqueous solution, the body of the sodium hydroxide solution and liquor zinci chloridi is then added dropwise
Product is than being 1:1, after ultrasonic mixing is uniform, it is slowly added to lauryl sodium sulfate, the lauryl sodium sulfate and zinc chloride
Mass ratio is 1:1, ultrasonic 2h, 160 DEG C of reaction 6h in reactor are moved to, is cleaned, centrifuged repeatedly with ethanol and deionized water, dried
Zinc oxide nanoparticle is obtained after processing.（3）PAMAM and zinc nitrate hexahydrate are configured to the water-soluble of 1g/L and 1mol/L respectively
Liquid, the volume ratio of PAMAM and the zinc nitrate hexahydrate aqueous solution is 1:1, after being mixed evenly, move to 200 in reactor
DEG C reaction 5h, cleaned repeatedly with ethanol and deionized water, centrifuge, Zinc oxide nanoparticle obtained after drying process.（4）By step
Zinc oxide nanoparticle in two is configured to the aqueous solution of mass fraction 1%, then impregnates the cationization cotton in step 1
The 30min in the nano zine oxide aqueous solution, bath raio 1:10, rinsed, dried repeatedly with deionized water after taking-up；Then by step 3
In Zinc oxide nanoparticle be configured to the aqueous solution of mass fraction 1%, above-mentioned cotton is immersed in the nano zine oxide aqueous solution
30min, bath raio 1:10, rinsed, dried repeatedly with deionized water after taking-up.（5）Above-mentioned cellulose fibre is placed in 80 DEG C, 1g/L
Graphene oxide water solution in 600min, bath raio 1:50, rinsed repeatedly with deionized water after taking-up, drying is obtained based on oxidation
The Multifunctional cellulose fiber of graphene/nanometer zinc oxide.
Embodiment 2：
（1）Flax is arranged in the sodium hydroxide solution that mass fraction is 20%, bath raio 1:50,90 DEG C of reaction 120min, spend
Ionized water is washed till neutrality repeatedly, and sodium hydroxide is obtained after drying and is modified linen；Then sodium hydroxide is modified linen again
It is scattered in deionized water, bath raio 1:50, add trimethylallylammonium chloride, wherein trimethylallylammonium chloride and hydrogen-oxygen
The mass ratio for changing sodium modification linen is 1:6,70 DEG C of reaction 12h, are cleaned, trimethyl alkene are obtained after drying repeatedly with deionized water
Propyl ammonium chloride is modified linen；Trimethylallylammonium chloride modification linen is scattered in deionized water again, bath raio
1:50, it is slowly added to the 10g/L polyamide-amide PAMAM aqueous solution, the PAMAM aqueous solution and trimethylallylammonium chloride
The volume ratio of the modified linen aqueous solution is 1:6,85 DEG C of reaction 90min, cleaning, drying obtains the linen that is cationized after taking-up.
（2）1mol/L liquor zinci chloridi is prepared, 1mol/L sodium hydrate aqueous solution, the sodium hydroxide solution is then added dropwise
Volume ratio with liquor zinci chloridi is 1:2, after ultrasonic mixing is uniform, it is slowly added to lauryl sodium sulfate, the dodecyl
The mass ratio of sodium sulphate and zinc chloride is 2:1, ultrasonic 2h, 160 DEG C of reaction 9h are moved in reactor, it is anti-with ethanol and deionized water
Zinc oxide nanoparticle is obtained after multiple cleaning, centrifugation, drying process.（3）PAMAM and zinc nitrate hexahydrate are configured to respectively
The 10g/L and 1mol/L aqueous solution, the volume ratio of PAMAM and the zinc nitrate hexahydrate aqueous solution is 2:1, it is mixed evenly
Afterwards, 200 DEG C of reaction 5h in reactor are moved to, cleaned repeatedly with ethanol and deionized water, centrifuge, zinc oxide is obtained after drying process
Nano particle.（4）Zinc oxide nanoparticle in step 2 is configured to the aqueous solution of mass fraction 2%, then by step 1
Cationization linen be immersed in 60min in the nano zine oxide aqueous solution, bath raio 1:10, rushed repeatedly with deionized water after taking-up
Wash, dry；Then Zinc oxide nanoparticle in step 3 is configured to the aqueous solution of mass fraction 2%, above-mentioned linen is soaked
Stain 60min in the nano zine oxide aqueous solution, bath raio 1:10, rinsed, dried, so far by one repeatedly with deionized water after taking-up
Layer nano zinc oxide is then repeated twice aforesaid operations to the surface of linen.（5）Above-mentioned cellulose fibre is placed in 80
DEG C, 300min in 10g/L graphene oxide water solution, bath raio 1:50, rinsed repeatedly with deionized water after taking-up, drying obtains
Multifunctional cellulose fiber based on graphene oxide/nano zine oxide.
Embodiment 3：
（1）Viscose fabric is placed in the sodium hydroxide solution that mass fraction is 20%, bath raio 1:50,90 DEG C of reaction 120min, are used
Deionized water is washed till neutrality repeatedly, and sodium hydroxide is obtained after drying and is modified viscose fabric；Then sodium hydroxide modification viscose glue is knitted
Thing is scattered in deionized water again, bath raio 1:50, add trimethylallylammonium chloride, wherein trimethylallylammonium chloride
The mass ratio that viscose fabric is modified with sodium hydroxide is 1:10,80 DEG C of reaction 24h, are cleaned repeatedly with deionized water, after drying
Viscose fabric is modified to trimethylallylammonium chloride；Trimethylallylammonium chloride modification viscose fabric is scattered in again
In ionized water, bath raio 1:50, it is slowly added to the 100g/L polyamide-amide PAMAM aqueous solution, the PAMAM aqueous solution and front three
The volume ratio that base allyl ammonium chloride is modified the viscose fabric aqueous solution is 1:5-1:10,95 DEG C of reaction 120min, are cleaned after taking-up
Drying obtains the viscose fabric that is cationized.（2）1mol/L liquor zinci chloridi is prepared, 1mol/L hydroxide is then added dropwise
Sodium water solution, the volume ratio of the sodium hydroxide solution and liquor zinci chloridi is 2:1, after ultrasonic mixing is uniform, it is slowly added to ten
The mass ratio of sodium dialkyl sulfate, the lauryl sodium sulfate and zinc chloride is 3:1, ultrasonic 2h, 160 DEG C are moved in reactor
12h is reacted, cleaned repeatedly with ethanol and deionized water, centrifuge, Zinc oxide nanoparticle is obtained after drying process.（3）By PAMAM
It is configured to 20g/L and the 1mol/L aqueous solution respectively with zinc nitrate hexahydrate, PAMAM and the zinc nitrate hexahydrate aqueous solution
Volume ratio is 5:1, after being mixed evenly, 200 DEG C of reaction 5h in reactor are moved to, cleaned repeatedly with ethanol and deionized water,
Zinc oxide nanoparticle is obtained after centrifugation, drying process.（4）Zinc oxide nanoparticle in step 2 is configured to mass fraction
5% aqueous solution, the cationization viscose fabric in step 1 is then immersed in 60min in the nano zine oxide aqueous solution, bath raio
1:10, rinsed, dried repeatedly with deionized water after taking-up；Then the Zinc oxide nanoparticle in step 3 is configured to quality point
The aqueous solution of number 5%, above-mentioned viscose fabric is immersed in 60min in the nano zine oxide aqueous solution, bath raio 1:10, spent after taking-up
Ionized water rinses repeatedly, drying, so far by one layer of nano zinc oxide to the surface of viscose fabric, then in triplicate on
State operation.（5）Above-mentioned cellulose fibre is placed in 80 DEG C, 60min in 20g/L graphene oxide water solution, bath raio 1:50, take
Rinsed repeatedly with deionized water after going out, drying obtains the Multifunctional cellulose fiber based on graphene oxide/nano zine oxide.
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 (7)
1. the preparation method of the Multifunctional cellulose fiber based on graphene oxide/nano zine oxide, it is characterised in that：
Step 1：Cellulose fibre is placed in the sodium hydroxide solution that mass fraction is 20%, bath raio 1:50,90 DEG C of reactions
120min, neutrality is washed till repeatedly with deionized water, sodium hydroxide modified cellulose fibre is obtained after drying；Then by sodium hydroxide
Modified cellulose fibre is scattered in deionized water again, bath raio 1:50, add trimethylallylammonium chloride, wherein trimethyl
The mass ratio of allyl ammonium chloride and sodium hydroxide modified cellulose fibre is 1:5-1:10,60-80 DEG C of reaction 1-24h, spend
Ionized water is cleaned repeatedly, and trimethylallylammonium chloride modified cellulose fibre is obtained after drying；By trimethyl allyl chlorination
Ammonium modified cellulose fibre is scattered in deionized water again, bath raio 1:50, it is slowly added to 1-100g/L polyamide-amide
The PAMAM aqueous solution, 75-95 DEG C of reaction 60-120min, cleaning, drying obtains cationized cellulose fiber after taking-up；
Step 2：1mol/L liquor zinci chloridi is prepared, 1mol/L sodium hydrate aqueous solution, ultrasonic mixing is then added dropwise
After uniformly, be slowly added to lauryl sodium sulfate, ultrasonic 2h, move to 160 DEG C of reaction 6-12h in reactor, with ethanol and go from
Sub- water cleans, centrifuges, Zinc oxide nanoparticle is obtained after drying process repeatedly；
Step 3：PAMAM and zinc nitrate hexahydrate are configured to 1-100g/L and the 1mol/L aqueous solution respectively, mixed equal
After even, 200 DEG C of reaction 5h in reactor are moved to, cleaned with ethanol and deionized water, centrifuge, aoxidized after drying process repeatedly
Zinc nanoparticles；
Step 4：Zinc oxide nanoparticle in step 2 is configured to the mass fraction 0.1-5% aqueous solution, then by step
Cationized cellulose fiber impregnation in one 30-60min, bath raio 1 in the nano zine oxide aqueous solution:10, spent after taking-up
Ionized water rinses repeatedly, drying；Then the Zinc oxide nanoparticle in step 3 is configured to the water-soluble of mass fraction 0.1-5%
Liquid, above-mentioned cellulose fibre is immersed in 30-60min in the nano zine oxide aqueous solution, bath raio 1:10, use deionized water after taking-up
Rinse, dry repeatedly, so far by one layer of nano zinc oxide to the surface of cellulose fibre, subsequent repeatedly aforesaid operations,
The number of plies of cellulose fiber surface nano zinc oxide is determined as needed；
Step 5：Above-mentioned cellulose fibre is placed in 80 DEG C, 60-600min in 1-20g/L graphene oxide water solution, bath raio
1:50, rinsed repeatedly with deionized water after taking-up, drying obtains the multifunctional fibre element based on graphene oxide/nano zine oxide
Fiber.
2. the preparation side of the Multifunctional cellulose fiber according to claim 1 based on graphene oxide/nano zine oxide
Method, it is characterised in that the cellulose fibre includes native cellulose fibre and regenerated celulose fibre.
3. the preparation side of the Multifunctional cellulose fiber according to claim 1 based on graphene oxide/nano zine oxide
Method, it is characterised in that the volume ratio of the PAMAM aqueous solution and the trimethylallylammonium chloride modified cellulose fibre aqueous solution
For 1:5-1:10.
4. the preparation side of the Multifunctional cellulose fiber according to claim 1 based on graphene oxide/nano zine oxide
Method, it is characterised in that the volume ratio of the sodium hydroxide solution and liquor zinci chloridi is 1:2-2:1.
5. the preparation side of the Multifunctional cellulose fiber according to claim 1 based on graphene oxide/nano zine oxide
Method, it is characterised in that the mass ratio of the lauryl sodium sulfate and zinc chloride is 1:1-3:1.
6. the preparation side of the Multifunctional cellulose fiber according to claim 1 based on graphene oxide/nano zine oxide
Method, it is characterised in that the volume ratio of PAMAM and the zinc nitrate hexahydrate aqueous solution is 1:1-5:1.
7. a kind of multifunctional fibre element based on graphene oxide/nano zine oxide obtained by claim 1 preparation method is fine
Dimension.
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| CN113699786A (en) * | 2021-10-14 | 2021-11-26 | 陈小琴 | Cotton fiber-based lasting antibacterial fiber fabric and preparation method thereof |
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