CN110424060A - A kind of preparation method of the carbon black modified viscose rayon of graphene/nanometer - Google Patents
A kind of preparation method of the carbon black modified viscose rayon of graphene/nanometer Download PDFInfo
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- CN110424060A CN110424060A CN201910837159.1A CN201910837159A CN110424060A CN 110424060 A CN110424060 A CN 110424060A CN 201910837159 A CN201910837159 A CN 201910837159A CN 110424060 A CN110424060 A CN 110424060A
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- carbon black
- graphene
- dbp value
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- 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
- D01F2/00—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof
- D01F2/06—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof from viscose
- D01F2/08—Composition of the spinning solution or the bath
Abstract
The invention discloses a kind of preparation methods of the carbon black modified viscose rayon of graphene/nanometer, by the way that the nano carbon black of specific DBP value is compound with single-layer graphene oxide with special ratios, graphene oxide occurs to restore and forms stable composite construction under the alkaline environment of heating, it can directly be mixed after washing with rayon spinning liquid, keep fine dispersion, it is obtained after spinning with antistatic, the New Viscose Fibre of UV resistance and antibacterial functions, product function is stable and does not decay with washing, it can be carried out directly on viscose fiber production line, it is minimum to original process variations, products obtained therefrom can be in underwear, housing, panty hose, it is applied in footwear material.
Description
Technical field
The invention belongs to the preparations of chemical & blended fabric field more particularly to a kind of carbon black modified viscose rayon of graphene/nanometer
Method.
Background technique
Viscose rayon category cellulose fibre.It is with natural fiber (wood-fibred, cotton linter) be raw material, through alkalization, aging,
Soluble cellulose xanthate is made in the processes such as sulfonation, is re-dissolved in sig water and viscose glue is made, and is made through wet spinning.Due to
Viscose rayon itself is extracted from natural lignose, with natural environmental-protective, hydrophilic ventilative, cool and comfortable characteristic.So
And as the improvement of people's living standards, propose new Functional Requirement to viscose rayon, such as UV resistance, fever, it is warming,
Antibacterial bacteriostatic, antistatic etc..It is whole after mainly passing through the various functional materials of addition to the modification of viscose rayon at present or passing through
Reason realizes above-mentioned function, has a single function, washing resistance performance and comfort are bad.
Graphene is newfound star's material in recent years, with impayable mechanics, electricity, calorifics, optics, is urged
Many performances such as change, semiconductor, it is considered to be " industrial monosodium glutamate " material of industrial upgrading can be caused.Surpass since graphene has
The heat subject for preparing antistatic or conductive material also and becoming in recent years is added in other materials in graphene by high conductivity.
Due to single layer and the number of plies it is few graphene price it is very expensive, existing market sale graphene modified fibre largely be addition
Grapheme material containing multi-layer graphene and graphite powder, graphene excellent performance does not find full expression, and valence
Lattice are high, limit its use scope.
CN109402815A " graphene composite fibre yarn and its preparation method and application " by graphene dispersion in water
Composite fibre is obtained with spinning viscose blend spinning, but graphene itself is not hydrophilic.Be difficult it is evenly dispersed in water, be unfavorable for
The realization of spinning and follow-up function.CN109440213A " a kind of graphene oxide modified flame-retardant cellulose fibre and its preparation side
Method " graphene oxide and fire retardant are mixed with first fibre after spinning, realize it is fire-retardant, enhancing and it is antibacterial.For viscose rayon,
The feature of its water phase preparation is particularly suitable for graphene oxide system, however for realizing anti-static effect, graphene oxide
Insulation characterisitic again be not suitable for.Therefore it needs to open up the preparation method of a kind of combination Aqueous dispersions and excellent conductive, solves viscose glue
The antistatic problem of fiber.
Summary of the invention
The purpose of the present invention is aiming at the shortcomings of the prior art, provide a kind of carbon black modified viscose rayon of graphene/nanometer
Preparation method.Constitute in the fiber of the fabric, redox graphene and carbon black it is compound after be dispersed in nylon-6 matrix body
Portion, and conductive network is formed, still conductivity can be kept unattenuated even across long-time service and washing, there is high durability.
The purpose of the present invention is what is be achieved through the following technical solutions: a kind of carbon black modified viscose fiber of graphene/nanometer
Preparation method, which comprises the following steps:
(1) 0.01 mass parts hydrogen-oxygen is added into 25 mass parts, the graphene oxide aqueous dispersions that mass concentration is 2mg/g
Change sodium to be mixed evenly, obtains mixed liquor；
(2) it after mixing the ratio of low DBP value nano carbon black and high DBP value nano carbon black 3~5:1 in mass ratio, obtains
Nano carbon black is mixed, 0.12~0.2 mass parts are mixed into nano carbon black and are added in step (1) resulting mixed liquor, at 100 DEG C
It is stirred to react 1h, obtains mixed dispersion liquid；The DBP value of the high DBP value nano carbon black is 360~400, low DBP value Nano carbon
Black DBP value is 200~280.
(3) 100 mass parts are added into mixed dispersion liquid obtained by step (2), the viscose glue that first fibre content is 9~12wt% is spun
Silk stock solution is shaped in coagulating bath by spinning head spinning after mixing, drawing-off, washing, desulfurization, oils, dries, being packaged
Obtain the carbon black modified viscose fiber of graphene/nanometer.
Further, the carbon-to-oxygen ratio of the graphene oxide of the step (1) is between 3 to 7.
The beneficial effects of the present invention are:
(1) one-step method is prepared for redox graphene/nano carbon black composite construction.In graphene oxide aqueous dispersions,
Nano carbon black meeting selective enrichment forms composite construction in modified graphene surface.Secondly, low DBP value carbon black has low structure
Degree, i.e., structure is partially fine and close, and porous structure is on the low side, can repair modified graphene surface defect, promotes the intrinsic electricity of modified graphene
Conductance, and the carbon black of high DBP value has the micro-structure more stretched, gap is flourishing, the meeting when being attached at modified graphene surface
It flexes outward, facilitates the formation of interface charge transmitting and conductive network.The present invention by adjusting modified graphene, height repeatedly
The proportion of DBP carbon black and low DBP carbon black, obtains optimum formula, the final anti-static effect (table 1) for realizing composite fibre.
(2) after sodium hydroxide heat-treats, the removing of surface of graphene oxide functional group, defect repaired, conductivity into
One step is promoted, however the graphene after restoring stable and uniform can still disperse in water.Nano carbon black is attached to reduction-oxidation graphite
Alkene surface is dispersed in water together, reduces the reunion of nano carbon black and graphene, and can be directly dispersing in rayon spinning liquid
It is formed jointly, easy to operate, dispersion effect is more excellent.
(3) graphene and carbon black are dispersed in viscose rayon intrinsic silicon, and form conductive network, even across long-term
Using and washing still can keep conductivity unattenuated, have high durability.
(4) addition of graphene and carbon black can also assign viscose rayon originally no performance, such as antibacterial, UV resistance.
(5) in fiber graphene content 0.56% hereinafter, nano carbon black total addition level is only 1%~2.2%, additive amount
Substantially less than market similar product and reported values, it is at low cost, it is easy to industrialized production.
To sum up, it is prepared simply using the composite fibre that this method obtains, antistatic performance is excellent, and durability is good, at low cost
It is honest and clean, there is significant advantage compared to traditional fibre, have a vast market foreground and application value.
Detailed description of the invention
Fig. 1 is the microcosmic composition schematic diagram of composite fibre, wherein 1 is single-layer graphene film, 2 lacking for graphene surface
It falls into, 3 be low degree of structuration carbon black, and 4 be high degree of structuration carbon black.
Specific embodiment
The present invention first mixes single-layer graphene oxide and nano carbon black with different DBP values in water, makes nanometer
Carbon black is selectively dispersed in defect area and the conjugation area of graphene oxide, under alkaline environment after heating reduction, graphene oxide
Surface oxygen functional group removing, defect are centainly repaired, so that graphene conjugated structure expands, improve its conductivity.And
Since thermokalite reduction wants low compared to reducing degree for thermal reduction and electronation, the graphene/nanometer carbon black after reduction
Composite construction in water still can stable and uniform dispersion.Gained redox graphene/nano carbon black aqueous dispersions can directly with
The mixing of rayon spinning liquid, continuously prepares through wet spinning technology with antistatic, antibacterial, the New Viscose Fibre of UV resistance.Stone
The carbon black of the low degree of structuration of black alkene on piece plays reparation defect, promotes the purpose of conductivity, the carbon black of high degree of structuration increases graphite
The interface interaction of alkene and cellulosic molecule, and facilitate the building (as shown in Figure 1) of conductive network.Product adds graphene and receives
Rice amounts of carbon black is low, and simple for process, industrial volume production difficulty is small, has significant market application value.
The present invention is specifically described below by embodiment, the present embodiment is served only for doing further the present invention
It is bright, it should not be understood as limiting the scope of the invention, those skilled in the art makes one according to the content of foregoing invention
A little nonessential changes and adjustment belong to protection scope of the present invention.
Embodiment 1:
(1) 0.01 mass parts hydrogen-oxygen is added into 25 mass parts, the graphene oxide aqueous dispersions that mass concentration is 2mg/g
Change sodium to be mixed evenly, obtain mixed liquor, wherein the carbon-to-oxygen ratio of graphene oxide is 3；
(2) step (1) institute is added in the low DBP value nano carbon black of 0.1 mass parts and the high DBP value nano carbon black of 0.02 mass parts
In the mixed liquor obtained, it is stirred to react 1h at 100 DEG C, obtains mixed dispersion liquid, wherein mixing nano carbon black gross weight is 0.12 matter
Part is measured, the DBP value of high DBP value nano carbon black is 380, and the DBP value of low DBP value nano carbon black is 200；
(3) 100 mass parts are added into mixed dispersion liquid obtained by step (2), the rayon spinning that first fibre content is 12wt%
Stoste is shaped in coagulating bath by spinning head spinning after mixing, drawing-off, washing, desulfurization, oils, dries, being packaged
To the carbon black modified viscose fiber of graphene/nanometer.
Through above step, the carbon black modified viscose fiber of graphene/nanometer is obtained, specific performance is as shown in table 1.
Embodiment 2:
(1) 0.01 mass parts hydrogen-oxygen is added into 25 mass parts, the graphene oxide aqueous dispersions that mass concentration is 2mg/g
Change sodium to be mixed evenly, obtain mixed liquor, wherein the carbon-to-oxygen ratio of graphene oxide is 3；
(2) step (1) is added in the low DBP value nano carbon black of 0.15 mass parts and the high DBP value nano carbon black of 0.05 mass parts
In resulting mixed liquor, it is stirred to react 1h at 100 DEG C, obtains mixed dispersion liquid, wherein mixing nano carbon black gross weight is 0.2 matter
Part is measured, the DBP value of high DBP value nano carbon black is 360, and the DBP value of low DBP value nano carbon black is 240；
(3) 100 mass parts are added into mixed dispersion liquid obtained by step (2), the rayon spinning that first fibre content is 12wt%
Stoste is shaped in coagulating bath by spinning head spinning after mixing, drawing-off, washing, desulfurization, oils, dries, being packaged
To the carbon black modified viscose fiber of graphene/nanometer.
Through above step, the carbon black modified viscose fiber of graphene/nanometer is obtained, specific performance is as shown in table 1.
Embodiment 3:
(1) 0.01 mass parts hydrogen-oxygen is added into 25 mass parts, the graphene oxide aqueous dispersions that mass concentration is 2mg/g
Change sodium to be mixed evenly, obtain mixed liquor, wherein the carbon-to-oxygen ratio of graphene oxide is 7；
(2) step (1) is added in the low DBP value nano carbon black of 0.03 mass parts and the high DBP value nano carbon black of 0.01 mass parts
In resulting mixed liquor, it is stirred to react 1h at 100 DEG C, obtains mixed dispersion liquid, wherein mixing nano carbon black gross weight is 0.04
Mass parts, the DBP value of high DBP value nano carbon black are 360, and the DBP value of low DBP value nano carbon black is 280；
(3) 100 mass parts are added into mixed dispersion liquid obtained by step (2), the rayon spinning that first fibre content is 12wt%
Stoste is shaped in coagulating bath by spinning head spinning after mixing, drawing-off, washing, desulfurization, oils, dries, being packaged
To the carbon black modified viscose fiber of graphene/nanometer.
Through above step, the carbon black modified viscose fiber of graphene/nanometer is obtained, specific performance is as shown in table 1.
Embodiment 4:
(1) 0.01 mass parts hydrogen-oxygen is added into 25 mass parts, the graphene oxide aqueous dispersions that mass concentration is 2mg/g
Change sodium to be mixed evenly, obtain mixed liquor, wherein the carbon-to-oxygen ratio of graphene oxide is 6；
(2) the low DBP value nano carbon black of 2 mass parts and the high DBP value nano carbon black of 0.4 mass parts are added obtained by step (1)
Mixed liquor in, be stirred to react 1h at 100 DEG C, obtain mixed dispersion liquid, wherein mixing nano carbon black gross weight be 2.4 mass
Part, the DBP value of high DBP value nano carbon black is 400, and the DBP value of low DBP value nano carbon black is 240；
(3) 100 mass parts are added into mixed dispersion liquid obtained by step (2), the rayon spinning that first fibre content is 12wt%
Stoste is shaped in coagulating bath by spinning head spinning after mixing, drawing-off, washing, desulfurization, oils, dries, being packaged
To the carbon black modified viscose fiber of graphene/nanometer.
Through above step, the carbon black modified viscose fiber of graphene/nanometer is obtained, specific performance is as shown in table 1.
Embodiment 5:
(1) 0.01 mass parts hydrogen-oxygen is added into 25 mass parts, the graphene oxide aqueous dispersions that mass concentration is 2mg/g
Change sodium to be mixed evenly, obtain mixed liquor, wherein the carbon-to-oxygen ratio of graphene oxide is 7；
(2) the high DBP value nano carbon black of 0.2 mass parts is added in step (1) resulting mixed liquor, is stirred at 100 DEG C
1h is reacted, mixed dispersion liquid is obtained, the DBP value of high DBP value nano carbon black is 380；
(3) 100 mass parts are added into mixed dispersion liquid obtained by step (2), the rayon spinning that first fibre content is 12wt%
Stoste is shaped in coagulating bath by spinning head spinning after mixing, drawing-off, washing, desulfurization, oils, dries, being packaged
To the carbon black modified viscose fiber of graphene/nanometer.
Through above step, the carbon black modified viscose fiber of graphene/nanometer is obtained, specific performance is as shown in table 1.
Embodiment 6:
(1) 0.01 mass parts hydrogen-oxygen is added into 25 mass parts, the graphene oxide aqueous dispersions that mass concentration is 2mg/g
Change sodium to be mixed evenly, obtain mixed liquor, wherein the carbon-to-oxygen ratio of graphene oxide is 3；
(2) the high DBP value nano carbon black of 0.2 mass parts is added in step (1) resulting mixed liquor, is stirred at 100 DEG C
1h is reacted, mixed dispersion liquid is obtained, the DBP value of low DBP value nano carbon black is 240；
(3) 100 mass parts are added into mixed dispersion liquid obtained by step (2), the rayon spinning that first fibre content is 12wt%
Stoste is shaped in coagulating bath by spinning head spinning after mixing, drawing-off, washing, desulfurization, oils, dries, being packaged
To the carbon black modified viscose fiber of graphene/nanometer.
Through above step, the carbon black modified viscose fiber of graphene/nanometer is obtained, specific performance is as shown in table 1.
Embodiment 7:
(1) 0.01 mass parts hydrogen-oxygen is added into 25 mass parts, the graphene oxide aqueous dispersions that mass concentration is 2mg/g
Change sodium to be mixed evenly, obtain mixed liquor, wherein the carbon-to-oxygen ratio of graphene oxide is 6；
(2) step (1) is added in the low DBP value nano carbon black of 0.15 mass parts and the high DBP value nano carbon black of 0.05 mass parts
In resulting mixed liquor, it is stirred to react 1h at 100 DEG C, obtains mixed dispersion liquid, wherein mixing nano carbon black gross weight is 0.2 matter
Part is measured, the DBP value of high DBP value nano carbon black is 360, and the DBP value of low DBP value nano carbon black is 240；
(3) 100 mass parts are added into mixed dispersion liquid obtained by step (2), the rayon spinning that first fibre content is 10wt%
Stoste is shaped in coagulating bath by spinning head spinning after mixing, drawing-off, washing, desulfurization, oils, dries, being packaged
To the carbon black modified viscose fiber of graphene/nanometer.
Through above step, the carbon black modified viscose fiber of graphene/nanometer is obtained, specific performance is as shown in table 1.
Embodiment 8:
(1) 0.01 mass parts hydrogen-oxygen is added into 25 mass parts, the graphene oxide aqueous dispersions that mass concentration is 2mg/g
Change sodium to be mixed evenly, obtain mixed liquor, wherein the carbon-to-oxygen ratio of graphene oxide is 3；
(2) step (1) is added in the low DBP value nano carbon black of 0.15 mass parts and the high DBP value nano carbon black of 0.05 mass parts
In resulting mixed liquor, it is stirred to react 1h at 100 DEG C, obtains mixed dispersion liquid, wherein mixing nano carbon black gross weight is 0.2 matter
Part is measured, the DBP value of high DBP value nano carbon black is 400, and the DBP value of low DBP value nano carbon black is 260；
(3) 100 mass parts are added into mixed dispersion liquid obtained by step (2), the rayon spinning original that first fibre content is 9wt%
Liquid is shaped in coagulating bath by spinning head spinning after mixing, drawing-off, washing, desulfurization, oils, dries, be packaged and obtain
The carbon black modified viscose fiber of graphene/nanometer.
Through above step, the carbon black modified viscose fiber of graphene/nanometer is obtained, specific performance is as shown in table 1.
Embodiment 9:
(1) 0.01 mass parts hydrogen-oxygen is added into 25 mass parts, the graphene oxide aqueous dispersions that mass concentration is 2mg/g
Change sodium to be mixed evenly, obtain mixed liquor, wherein the carbon-to-oxygen ratio of graphene oxide is 6；
(2) step (1) is added in the low DBP value nano carbon black of 0.15 mass parts and the high DBP value nano carbon black of 0.05 mass parts
In resulting mixed liquor, it is stirred to react 1h at 100 DEG C, obtains mixed dispersion liquid, wherein mixing nano carbon black gross weight is 0.2 matter
Part is measured, the DBP value of high DBP value nano carbon black is 500, and the DBP value of low DBP value nano carbon black is 100；
(3) 100 mass parts are added into mixed dispersion liquid obtained by step (2), the rayon spinning that first fibre content is 12wt%
Stoste is shaped in coagulating bath by spinning head spinning after mixing, drawing-off, washing, desulfurization, oils, dries, being packaged
To the carbon black modified viscose fiber of graphene/nanometer.
Through above step, the carbon black modified viscose fiber of graphene/nanometer is obtained, specific performance is as shown in table 1.
The relevant parameter and composite fibre performance of 1 embodiment of table
It can be seen that from the comparison of embodiment 1-4 as nano carbon black additive amount is promoted in a certain range, composite fibre
Resistivity further decreases, and antibiotic property and uv resistance are also promoted.But when adding too much (embodiment 4), nano carbon black is certainly
Agglomeration is obvious, and composite fibre spinnability reduces, and resistivity is also higher.Conversely, (embodiment when nano carbon black additive amount is too low
3), the effect of carbon black is unobvious, and fabric resistor rate is excessively high, and bacteriostasis rate and UV resistance coefficient also decrease.
Embodiment 5,6 proves, high DBP nano carbon black is used alone or low DBP nano carbon black all cannot achieve composite fibre
Effective conductance only realize two kinds of " defect repair " and " network is formed " simultaneously this is because lacking the mechanism of synergistic effect
Effect could realize that conductivity significantly rise under the addition of low carbon black, otherwise still need to largely to add carbon black and be just able to achieve similar effect
Fruit.
It is found that as viscose glue original liquid concentration reduces, graphene/nanometer carbon black adds the comparison of embodiment 2,7,8 in the fibre
Amount rises, and resistivity decreases, antibiotic property and UV resistance performance boost.But adding too much graphene and carbon black reunion add
Play, difficulty in spinning, on the contrary additive amount crosses low-function and is difficult to embody.
Embodiment 9 is then to have selected the progress of the nano carbon black of higher DBP value and lower DBP value compound, and effect is still inferior to this
It is that invention claim obtains as a result, this is because the nano carbon black of lower DBP value itself to form conductive network ability poor, and repair
The effect of multiple modified graphene defect is worse, and the nano carbon black dispersion effect of excessively high DBP value is bad, and easy reunion causes.
Claims (2)
1. a kind of preparation method of the carbon black modified viscose fiber of graphene/nanometer, which comprises the following steps:
(1) 0.01 mass parts sodium hydroxide is added into 25 mass parts, the graphene oxide aqueous dispersions that mass concentration is 2mg/g
It is mixed evenly, obtains mixed liquor；
(2) it after mixing the ratio of low DBP value nano carbon black and high DBP value nano carbon black 3~5:1 in mass ratio, is mixed
0.12~0.2 mass parts are mixed nano carbon black and are added in step (1) resulting mixed liquor, stirred at 100 DEG C by nano carbon black
1h is reacted, mixed dispersion liquid is obtained；The DBP value of the high DBP value nano carbon black is 360~400, low DBP value nano carbon black
DBP value is 200~280.
(3) 100 mass parts are added into mixed dispersion liquid obtained by step (2), the rayon spinning original that first fibre content is 9~12wt%
Liquid is shaped in coagulating bath by spinning head spinning after mixing, drawing-off, washing, desulfurization, oils, dries, be packaged and obtain
The carbon black modified viscose fiber of graphene/nanometer.
2. the method according to claim 1, wherein the carbon-to-oxygen ratio of graphene oxide described in step (1) is arrived 3
Between 7.
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| CN115821409A (en) * | 2022-10-26 | 2023-03-21 | 赛得利(江苏)纤维有限公司 | Method for improving blackness of stock solution coloring viscose fibers |
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