CN110172747A - A kind of gold graphene oxide regenerated cellulose composite fibre and preparation method thereof - Google Patents
A kind of gold graphene oxide regenerated cellulose composite fibre and preparation method thereof Download PDFInfo
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- CN110172747A CN110172747A CN201910374563.XA CN201910374563A CN110172747A CN 110172747 A CN110172747 A CN 110172747A CN 201910374563 A CN201910374563 A CN 201910374563A CN 110172747 A CN110172747 A CN 110172747A
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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 golden graphene oxide regenerated cellulose composite fibres and preparation method thereof, raw material includes: regenerated cellulose compound pulp 60~84.9%, graphene oxide solution 0.1~10%, surfactant 0.1~5%, alkaline reagent 0.1~5%, surplus are water.Preparation method includes: step 1, weighing raw material；Step 2, graphene oxide powder is prepared；Step 3, graphene oxide solution is configured, surfactant and alkaline reagent, ultrasonic disperse are added；Step 4, regenerated cellulose compound pulp is weighed, is mixed with sodium hydroxide solution, is squeezed；Experienced processing is carried out again；Then yellow；Step 5, graphene oxide mixed solution is heated up, is mixed with pulp, stirred；Step 6, spinning is carried out.The composite fibre with the functions such as antibacterial, anti-mite, uvioresistant, far infrared of gold prepared by the present invention, is able to ascend regenerated cellulose composite fibre added value, extends its use scope.
Description
Technical field
The present invention relates to a kind of composite fibres and preparation method thereof, and in particular, to a kind of gold graphene oxide regeneration
Cellulose composite fiber and preparation method thereof.
Background technique
Graphene is the single layer of carbon atom material being stripped out from graphite, tightly packed at single layer two dimension bee by carbon atom
Nest shape lattice structure, it is the material that thickness known to the mankind is most thin, quality is most hard, electric conductivity is best.Graphene has excellent
Different mechanics, electrical and optical properties, structure is highly stable, and researcher not yet has found have carbon atom to lack in graphene so far
The case where mistake, the link between carbon atom is very flexible, also harder than diamond, on the intensity steel more best than in the world is taller
100 times, if packaging bag is made with graphene, it will bear about two tons of heavy articles, almost transparent, but extremely cause
It is close, it is waterproof, airtight, it can not pass through atomic size the smallest helium, conduct electricity very well, the fortune of electronics in graphene
Dynamic speed has reached the 1/300 of the light velocity, and electric conductivity has been more than any traditional conductive material, chemical property similar to graphite surface,
Various atoms and molecule can be adsorbed and be desorbed, the ability of strong acid and strong base is also resisted.
Graphene oxide has carboxyl, epoxy group, the modification of the oxygen-containing groups such as hydroxyl on the surface layer of graphene.Due to aoxidizing stone
Black alkene preparation process is simpler, and the cost of raw material is cheap, at the same in practical operation graphene oxide compared with graphene less
It is easy to reunite, therefore can be widely applied in large-scale industrial production.
Regenerated cellulose composite fibre is a kind of cellulose fibre that purposes is relatively broad, itself has good mechanical property
Energy, hygroscopicity, but do not have functionality.Traditional functional regenerated cellulose composite fibre is mainly by fine in regeneration
It ties up and adds auxiliary agent in plain composite fibre or by realizing to fibre modification, and the regenerated cellulose of this method preparation is multiple
Condensating fiber, functional intolerant to washing, pollution caused by post-processing is more serious, therefore makes regenerated cellulose composite fibre application
It is subject to certain restrictions.
Summary of the invention
The object of the present invention is to provide a kind of composite fibres and preparation method thereof, molten using improved golden graphene oxide
It is fine that liquid preparation and dispersion and improved regenerated cellulose compound pulp system prepare a kind of golden graphene oxide regeneration
Plain composite fibre is tieed up, which has gold, and spinning and weaving can directly be carried out by being not required to dyeing, while the regenerated cellulose is multiple
Condensating fiber has the functions such as antibacterial, anti-mite, far infrared, uvioresistant, extends regenerated celulose fibre application range.
In order to achieve the above object, the present invention provides a kind of golden graphene oxide regenerated cellulose composite fibre,
In, the raw material of the composite fibre includes by mass percentage: regenerated cellulose compound pulp 60%~84.9%, oxidation
Graphene solution 0.1%~10%, surfactant 0.1%~5%, alkaline reagent 0.1%~5%, surplus are water.
Above-mentioned golden graphene oxide regenerated cellulose composite fibre, wherein the surfactant is to include wood
Quality sodium sulfonate, polyethylene pyrrole network alkanone (PVP), neopelex mixture.
Above-mentioned golden graphene oxide regenerated cellulose composite fibre, wherein lignin in the surfactant
Sodium sulfonate, polyethylene pyrrole network alkanone, neopelex mass ratio be 1:(1~3): (2~5).
Above-mentioned golden graphene oxide regenerated cellulose composite fibre, wherein the alkaline reagent includes ammonium hydroxide, hydrogen
Potassium oxide, any one or more in sodium hydroxide.
The present invention also provides the preparation methods of above-mentioned golden graphene oxide regenerated cellulose composite fibre, wherein
The method includes: step 1, weighing each raw material in proportion；Step 2, graphene oxide powder is prepared；Step 3, by step 2
Graphene oxide powder obtained is soluble in water, configures graphene oxide solution, and add surfactant and alkaline reagent, will
Solution is adjusted to neutral or alkalescent to be made it be uniformly dispersed, obtains graphene oxide mixed solution then by its ultrasound；Step
4, regenerated cellulose compound pulp is weighed, it is mixed with sodium hydroxide solution, stirs, is thoroughly mixed it；Then it is pressed
It squeezes；Pulp is subjected to experienced processing again；Yellow is carried out after the completion of experienced processing；Step 5, by graphite oxide made from step 3
The heating of alkene mixed solution, then mixes with the resulting pulp of step 4, stirs, obtains regenerated cellulose composite fibre pulp；Step
6, regenerated cellulose composite fibre pulp made from step 5 is subjected to spinning, it is multiple to prepare golden graphene oxide regenerated cellulose
Condensating fiber.
The preparation method of above-mentioned golden graphene oxide regenerated cellulose composite fibre, wherein the step 2 uses
Hummers method prepares graphene oxide, includes: step 2.1, into the 1000ml reaction flask being placed in water-bath be added 100~
The dense H that 300ml mass concentration is 98%2SO4；Weigh 5g graphite powder and 2g NaNO respectively again3Solid, add it to reaction
In bottle, turn on agitator stirs 30min；KMnO is added after stirring415g, control reaction temperature are equal to or less than 25 DEG C,
Stir 15min；Water-bath is warming up to 30~40 DEG C, continues stir about 1h；Stirring terminates the temperature of water-bath being warming up to 90
DEG C, 300ml deionized water is instilled in solution；The H that 200~500ml mass concentration is 30% is measured simultaneously2O2, it is added to solution
In, solution becomes vivid yellow from brownish black；Continue to stir 10min, then solution is poured into beaker, 5~15min of ultrasound；
It is finally filtered, is then sufficiently filtered with deionized water again until in filtrate with the dilute hydrochloric acid that the mass concentration of 1000ml is 5.5%
Until sulfate radical-free ion；Step 2.2, the resulting product of step 2.1 is dried using freeze drier, is obtained spongy
Graphene oxide；The graphene oxide of acquisition is put into airslide disintegrating mill again to crush, grinding time is 1~3 hour, is aoxidized
Graphene powder.
The preparation method of above-mentioned golden graphene oxide regenerated cellulose composite fibre, wherein the step 2 is made
Graphene oxide powder partial size D90 less than 10 μm.
The preparation method of above-mentioned golden graphene oxide regenerated cellulose composite fibre, wherein in the step 3,
Graphene oxide powder is dissolved in deionized water, configuration concentration is the graphene oxide solution of 1~50mg/ml, and in proportion
Surfactant and alkaline reagent are added, solution is adjusted to neutral or alkalescent to be made then by its ultrasound 10min~30min
It is uniformly dispersed.
The preparation method of above-mentioned golden graphene oxide regenerated cellulose composite fibre, wherein in the step 4,
The compound cellulose pulp of regenerated cellulose is prepared, 500g regenerated cellulose compound pulp is weighed, by it according to mass ratio 1:(2
~4) sodium hydroxide solution for being 20%~40% with mass concentration mixes, and blender stirs 20~50min, keeps it completely mixed
It closes；Then it puts it into squeezer and squeezes, set pressure as 2~6kpa, the squeezing time is 10~30min；Again by pulp into
The experienced processing of row, experienced temperature are 20~25 DEG C, and the time is 3~5h, then temperature is risen to 30~35 DEG C, continue aging, aging
Time is 1~3h；Carry out yellow after the completion of experienced processing, 20~25 DEG C of yellow temperature, 20~30min of yellow time, then will
Temperature rises to 25~30 DEG C, continues yellow, the time is also 20~30min.
The preparation method of above-mentioned golden graphene oxide regenerated cellulose composite fibre, wherein in the step 5,
Graphene oxide mixed solution is warming up to 25~30 DEG C, then mixes with pulp, is stirred using blender in proportion, the time is
20~50min obtains regenerated cellulose composite fibre pulp, wherein graphene oxide solid content and pulp fibers element solid content
Ratio is (0.01~5) %:1.
Gold graphene oxide regenerated cellulose composite fibre provided by the invention and preparation method thereof has the advantage that
The present invention develops graphene regenerated cellulose composite fibre, the composite fibre appearance outstanding feature be have it is bright
Aobvious gold, beautiful appearance, while composite fibre also have the performances such as antibacterial, anti-mite, far infrared, uvioresistant, and functionality is resistance to
Washing, is not required to independent aftertreatment technology, safety and environmental protection better meets current people to functionality, comfort, healthy textile
Requirement.
The method comprises the steps of firstly, preparing graphene oxide solutions that can be evenly dispersed, and by graphene oxide solution by certain
Ratio is added in regenerated cellulose compound pulp, prepares golden graphene regenerated cellulose using improved wet spinning technology
Composite fibre.Composite fibre antibacterial, anti-mite, far infrared, the function admirables such as uvioresistant of this method preparation, wherein Escherichia coli,
Gold-coloured staphylococci, Candida albicans bacteriostasis rate reach 99.9%, and suppression mite rate is greater than 90%, and far-infrared temperature rise reaches 0.88, UPF
It is functional good greater than 100.
The graphene regenerated cellulose composite fibre of this method preparation, simple process is easy to operate, low in cost, economic benefit
Height is suitble to large-scale industrial production.
Specific embodiment
A specific embodiment of the invention is further described below.
Gold graphene oxide regenerated cellulose composite fibre provided by the invention, raw material wrap by mass percentage
Contain: regenerated cellulose compound pulp 60%~84.9%, graphene oxide solution 0.1%~10%, surfactant 0.1%~
5%, alkaline reagent 0.1%~5%, surplus is water.
Regenerated celulose fibre (cellulose fiber) is to be with native cellulose (cotton, fiber crops, bamboo, tree, shrub etc.)
Raw material does not change its chemical structure, only changes the physical structure of native cellulose, to manufacture performance preferably again
Raw cellulose fibre.Regenerated cellulose compound pulp is that cotton, fiber crops, bamboo, tree, shrub etc. is used to form for raw material combined processing
Cellulose pulp.
Preferably, surfactant is to include sodium lignin sulfonate, polyethylene pyrrole network alkanone (PVP), detergent alkylate sulphur
The mixture of sour sodium.
Sodium lignin sulfonate in surfactant, polyethylene pyrrole network alkanone, neopelex mass ratio be 1:
(1~3): (2~5).
Alkaline reagent includes ammonium hydroxide, potassium hydroxide, any one or more in sodium hydroxide.
The present invention also provides the preparation method of the gold graphene oxide regenerated cellulose composite fibre, it includes: step
Rapid 1, each raw material is weighed in proportion；Step 2, graphene oxide powder is prepared；Step 3, by graphene oxide powder made from step 2
Body is soluble in water, configures graphene oxide solution, and add surfactant and alkaline reagent, and solution is adjusted to neutral or weak
Alkalinity makes it be uniformly dispersed, obtains graphene oxide mixed solution then by its ultrasound；Step 4, it is multiple to weigh regenerated cellulose
Pulp is closed, it is mixed with sodium hydroxide solution, stirs, is thoroughly mixed it；Then it is squeezed；Pulp is carried out again experienced
Processing；Yellow is carried out after the completion of experienced processing；Step 5, graphene oxide mixed solution made from step 3 is heated up, then
It is mixed with the resulting pulp of step 4, stirs, obtain regenerated cellulose composite fibre pulp；Step 6, it will be regenerated made from step 5
Cellulose composite fiber pulp carries out spinning, prepares golden graphene oxide regenerated cellulose composite fibre.Spinning technique and ginseng
Number etc. is all made of the routine techniques in this field.
Preferably, step 2 prepares graphene oxide using Hummers method, it includes: step 2.1, to being placed in water-bath
1000ml reaction flask in be added 100~300ml mass concentration be 98% dense H2SO4；Weigh 5g graphite powder and 2g respectively again
NaNO3Solid, add it in reaction flask, turn on agitator stir 30min；KMnO is added after stirring415g, control
Reaction temperature processed is equal to or less than 25 DEG C, stirs 15min；Water-bath is warming up to 30~40 DEG C, continues stir about 1h；Stirring knot
The temperature of water-bath is warming up to 90 DEG C by beam, and 300ml deionized water is instilled in solution；It is dense that 200~500ml mass is measured simultaneously
The H that degree is 30%2O2, it is added in solution, solution becomes vivid yellow from brownish black；Continue to stir 10min, then by solution
It pours into beaker, 5~15min of ultrasound；It is finally filtered with the dilute hydrochloric acid that the mass concentration of 1000ml is 5.5%, is then spent again
Ionized water sufficiently filters until sulfate radical-free ion in filtrate；Step 2.2, using freeze drier to obtained by step 2.1
Product be dried, obtain spongy graphene oxide；The graphene oxide of acquisition is put into airslide disintegrating mill again to crush, powder
The broken time is 1~3 hour, obtains graphene oxide powder.
The partial size D90 of graphene oxide powder made from step 2 is less than 10 μm.
In step 3, graphene oxide powder is dissolved in deionized water, configuration concentration is the graphite oxide of 1~50mg/ml
Alkene solution, and surfactant and alkaline reagent are added in proportion, solution is adjusted to neutral or alkalescent, then by its ultrasound
10min~30min makes it be uniformly dispersed.
In step 4, the compound cellulose pulp of regenerated cellulose is prepared, 500g regenerated cellulose compound pulp is weighed, it will
It is according to mass ratio 1:(2~4) it is mixed with mass concentration for 20%~40% sodium hydroxide solution, blender stirring 20~
50min is thoroughly mixed it；Then it putting it into squeezer and squeezes, set pressure as 2~6kpa, the squeezing time is 10~
30min；Pulp is subjected to experienced processing again, experienced temperature is 20~25 DEG C, and the time is 3~5h, then temperature is risen to 30~35
DEG C, continue aging, ageing time is 1~3h；Carry out yellow after the completion of experienced processing, 20~25 DEG C of yellow temperature, when yellow
Between 20~30min, then temperature is risen to 25~30 DEG C, continues yellow, the time is also 20~30min.
In step 5, graphene oxide mixed solution is warming up to 25~30 DEG C, is then mixed in proportion with pulp, used
Blender stirring, the time be 20~50min, obtain regenerated cellulose composite fibre pulp, wherein graphene oxide solid content with
The ratio of pulp fibers element solid content is (0.01~5) %:1.
Below with reference to embodiment to golden graphene oxide regenerated cellulose composite fibre provided by the invention and its preparation
Method is further described.
Embodiment 1
A kind of gold graphene oxide regenerated cellulose composite fibre, raw material includes by mass percentage: regeneration is fine
The plain compound pulp 84.9% of dimension, graphene oxide solution 0.1%, surfactant 0.1%, alkaline reagent 0.1%, surplus are
Water.
Preferably, surfactant is to include sodium lignin sulfonate, polyethylene pyrrole network alkanone (PVP), detergent alkylate sulphur
The mixture of sour sodium.
Sodium lignin sulfonate, polyethylene pyrrole network alkanone, neopelex mass ratio be 1:1:2.
Alkaline reagent includes ammonium hydroxide.
The present embodiment additionally provides the preparation method of the gold graphene oxide regenerated cellulose composite fibre, it includes:
Step 1, each raw material is weighed in proportion.
Step 2, graphene oxide powder is prepared.
Preferably, graphene oxide is prepared using Hummers method, includes:
Step 2.1, into the 1000ml reaction flask being placed in water-bath be added 100ml mass concentration be 98% it is dense
H2SO4；Weigh 5g graphite powder and 2g NaNO respectively again3Solid, add it in reaction flask, turn on agitator stirring
30min；KMnO is added after stirring415g, control reaction temperature are equal to or less than 25 DEG C, stir 15min；By water-bath liter
Temperature continues stir about 1h to 30~40 DEG C；Stirring terminates the temperature of water-bath being warming up to 90 DEG C, by 300ml deionized water drop
Enter in solution；The H that 200ml mass concentration is 30% is measured simultaneously2O2, it is added in solution, solution becomes vivid from brownish black
Yellow；Continue to stir 10min, then solution is poured into beaker, 5~15min of ultrasound；Finally it is with the mass concentration of 1000ml
5.5% dilute hydrochloric acid filtering, is then sufficiently filtered until sulfate radical-free ion in filtrate with deionized water again.
Step 2.2, the resulting product of step 2.1 is dried using freeze drier, obtains spongy graphite oxide
Alkene；The graphene oxide of acquisition is put into airslide disintegrating mill again to crush, grinding time is 1~3 hour, obtains graphene oxide powder
Body.The partial size D90 of its graphene oxide powder obtained is less than 10 μm.
Step 3, graphene oxide powder made from step 2 is dissolved in deionized water, configuration concentration is the oxygen of 1mg/ml
Graphite alkene solution, and surfactant and alkaline reagent are added in proportion, solution is adjusted to neutral or alkalescent, then will
Its ultrasound 10min~30min, makes it be uniformly dispersed, obtains graphene oxide mixed solution.
Step 4, prepare that regenerated cellulose is compound to use cellulose pulp.
Weigh 500g regenerated cellulose compound pulp, by its be 20% according to mass ratio 1:2 and mass concentration hydroxide
Sodium solution mixing, blender stir 20~50min, are thoroughly mixed it；Then it puts it into squeezer and squeezes, set pressure
For 2~6kpa, the squeezing time is 10~30min；Pulp is subjected to experienced processing again, experienced temperature is 20~25 DEG C, the time 3
~5h, then temperature is risen to 30~35 DEG C, continue aging, ageing time is 1~3h；Yellow is carried out after the completion of experienced processing,
20~25 DEG C of yellow temperature, 20~30min of yellow time, then temperature is risen to 25~30 DEG C, continue yellow, the time is also 20~
30min。
Step 5, graphene oxide mixed solution made from step 3 is warming up to 25~30 DEG C, then in proportion with step 4
Resulting pulp mixing, is stirred using blender, and the time is 20~50min, obtains regenerated cellulose composite fibre pulp, wherein
The ratio of graphene oxide solid content and pulp fibers element solid content is (0.01~5) %:1, obtains the compound fibre of regenerated cellulose
Tie up pulp.
Step 6, regenerated cellulose composite fibre pulp made from step 5 is subjected to spinning, prepares golden graphene oxide
Regenerated cellulose composite fibre.
Embodiment 2
A kind of gold graphene oxide regenerated cellulose composite fibre, raw material includes by mass percentage: regeneration is fine
Plain compound pulp 80% is tieed up, graphene oxide solution 3%, surfactant 1.5%, alkaline reagent 1%, surplus is water.
Preferably, surfactant is to include sodium lignin sulfonate, polyethylene pyrrole network alkanone (PVP), detergent alkylate sulphur
The mixture of sour sodium.
Sodium lignin sulfonate, polyethylene pyrrole network alkanone, neopelex mass ratio be 1:1.5:3.
Alkaline reagent includes potassium hydroxide.
The present embodiment additionally provides the preparation method of the gold graphene oxide regenerated cellulose composite fibre, it includes:
Step 1, each raw material is weighed in proportion.
Step 2, graphene oxide powder is prepared.
Preferably, graphene oxide is prepared using Hummers method, includes:
Step 2.1, into the 1000ml reaction flask being placed in water-bath be added 150ml mass concentration be 98% it is dense
H2SO4；Weigh 5g graphite powder and 2g NaNO respectively again3Solid, add it in reaction flask, turn on agitator stirring
30min；KMnO is added after stirring415g, control reaction temperature are equal to or less than 25 DEG C, stir 15min；By water-bath liter
Temperature continues stir about 1h to 30~40 DEG C；Stirring terminates the temperature of water-bath being warming up to 90 DEG C, by 300ml deionized water drop
Enter in solution；The H that 250ml mass concentration is 30% is measured simultaneously2O2, it is added in solution, solution becomes vivid from brownish black
Yellow；Continue to stir 10min, then solution is poured into beaker, 5~15min of ultrasound；Finally it is with the mass concentration of 1000ml
5.5% dilute hydrochloric acid filtering, is then sufficiently filtered until sulfate radical-free ion in filtrate with deionized water again.
Step 2.2, the resulting product of step 2.1 is dried using freeze drier, obtains spongy graphite oxide
Alkene；The graphene oxide of acquisition is put into airslide disintegrating mill again to crush, grinding time is 1~3 hour, obtains graphene oxide powder
Body.The partial size D90 of its graphene oxide powder obtained is less than 10 μm.
Step 3, graphene oxide powder made from step 2 is dissolved in deionized water, configuration concentration is the oxygen of 15mg/ml
Graphite alkene solution, and surfactant and alkaline reagent are added in proportion, solution is adjusted to neutral or alkalescent, then will
Its ultrasound 10min~30min, makes it be uniformly dispersed, obtains graphene oxide mixed solution.
Step 4, prepare that regenerated cellulose is compound to use cellulose pulp.
Weigh 500g regenerated cellulose compound pulp, by its be 25% according to mass ratio 1:2.5 and mass concentration hydrogen-oxygen
Change sodium solution mixing, blender stirs 20~50min, is thoroughly mixed it；Then it puts it into squeezer and squeezes, setting pressure
Power is 2~6kpa, and the squeezing time is 10~30min；Pulp is subjected to experienced processing again, experienced temperature is 20~25 DEG C, the time
For 3~5h, then temperature risen to 30~35 DEG C, continues aging, ageing time is 1~3h；It is carried out after the completion of experienced processing yellow
Change, 20~25 DEG C of yellow temperature, 20~30min of yellow time, then temperature is risen to 25~30 DEG C, continue yellow, the time is also
20~30min.
Step 5, graphene oxide mixed solution made from step 3 is warming up to 25~30 DEG C, then in proportion with step 4
Resulting pulp mixing, is stirred using blender, and the time is 20~50min, obtains regenerated cellulose composite fibre pulp, wherein
The ratio of graphene oxide solid content and pulp fibers element solid content is (0.01~5) %:1, obtains the compound fibre of regenerated cellulose
Tie up pulp.
Step 6, regenerated cellulose composite fibre pulp made from step 5 is subjected to spinning, prepares golden graphene oxide
Regenerated cellulose composite fibre.
Embodiment 3
A kind of gold graphene oxide regenerated cellulose composite fibre, raw material includes by mass percentage: regeneration is fine
Plain compound pulp 70% is tieed up, graphene oxide solution 5%, surfactant 2%, alkaline reagent 3%, surplus is water.
Preferably, surfactant is to include sodium lignin sulfonate, polyethylene pyrrole network alkanone (PVP), detergent alkylate sulphur
The mixture of sour sodium.
Sodium lignin sulfonate, polyethylene pyrrole network alkanone, neopelex mass ratio be 1:2:3.5.
Alkaline reagent includes sodium hydroxide.
The present embodiment additionally provides the preparation method of the gold graphene oxide regenerated cellulose composite fibre, it includes:
Step 1, each raw material is weighed in proportion.
Step 2, graphene oxide powder is prepared.
Preferably, graphene oxide is prepared using Hummers method, includes:
Step 2.1, into the 1000ml reaction flask being placed in water-bath be added 200ml mass concentration be 98% it is dense
H2SO4；Weigh 5g graphite powder and 2g NaNO respectively again3Solid, add it in reaction flask, turn on agitator stirring
30min；KMnO is added after stirring415g, control reaction temperature are equal to or less than 25 DEG C, stir 15min；By water-bath liter
Temperature continues stir about 1h to 30~40 DEG C；Stirring terminates the temperature of water-bath being warming up to 90 DEG C, by 300ml deionized water drop
Enter in solution；The H that 350ml mass concentration is 30% is measured simultaneously2O2, it is added in solution, solution becomes vivid from brownish black
Yellow；Continue to stir 10min, then solution is poured into beaker, 5~15min of ultrasound；Finally it is with the mass concentration of 1000ml
5.5% dilute hydrochloric acid filtering, is then sufficiently filtered until sulfate radical-free ion in filtrate with deionized water again.
Step 2.2, the resulting product of step 2.1 is dried using freeze drier, obtains spongy graphite oxide
Alkene；The graphene oxide of acquisition is put into airslide disintegrating mill again to crush, grinding time is 1~3 hour, obtains graphene oxide powder
Body.The partial size D90 of its graphene oxide powder obtained is less than 10 μm.
Step 3, graphene oxide powder made from step 2 is dissolved in deionized water, configuration concentration is the oxygen of 25mg/ml
Graphite alkene solution, and surfactant and alkaline reagent are added in proportion, solution is adjusted to neutral or alkalescent, then will
Its ultrasound 10min~30min, makes it be uniformly dispersed, obtains graphene oxide mixed solution.
Step 4, prepare that regenerated cellulose is compound to use cellulose pulp.
Weigh 500g regenerated cellulose compound pulp, by its be 30% according to mass ratio 1:3 and mass concentration hydroxide
Sodium solution mixing, blender stir 20~50min, are thoroughly mixed it；Then it puts it into squeezer and squeezes, set pressure
For 2~6kpa, the squeezing time is 10~30min；Pulp is subjected to experienced processing again, experienced temperature is 20~25 DEG C, the time 3
~5h, then temperature is risen to 30~35 DEG C, continue aging, ageing time is 1~3h；Yellow is carried out after the completion of experienced processing,
20~25 DEG C of yellow temperature, 20~30min of yellow time, then temperature is risen to 25~30 DEG C, continue yellow, the time is also 20~
30min。
Step 5, graphene oxide mixed solution made from step 3 is warming up to 25~30 DEG C, then in proportion with step 4
Resulting pulp mixing, is stirred using blender, and the time is 20~50min, obtains regenerated cellulose composite fibre pulp, wherein
The ratio of graphene oxide solid content and pulp fibers element solid content is (0.01~5) %:1, obtains the compound fibre of regenerated cellulose
Tie up pulp.
Step 6, regenerated cellulose composite fibre pulp made from step 5 is subjected to spinning, prepares golden graphene oxide
Regenerated cellulose composite fibre.
Embodiment 4
A kind of gold graphene oxide regenerated cellulose composite fibre, raw material includes by mass percentage: regeneration is fine
Plain compound pulp 65% is tieed up, graphene oxide solution 7%, surfactant 4%, alkaline reagent 4%, surplus is water.
Preferably, surfactant is to include sodium lignin sulfonate, polyethylene pyrrole network alkanone (PVP), detergent alkylate sulphur
The mixture of sour sodium.
Sodium lignin sulfonate, polyethylene pyrrole network alkanone, neopelex mass ratio be 1:2.5:4.
Alkaline reagent includes potassium hydroxide or sodium hydroxide.
The present embodiment additionally provides the preparation method of the gold graphene oxide regenerated cellulose composite fibre, it includes:
Step 1, each raw material is weighed in proportion.
Step 2, graphene oxide powder is prepared.
Preferably, graphene oxide is prepared using Hummers method, includes:
Step 2.1, into the 1000ml reaction flask being placed in water-bath be added 250ml mass concentration be 98% it is dense
H2SO4；Weigh 5g graphite powder and 2g NaNO respectively again3Solid, add it in reaction flask, turn on agitator stirring
30min；KMnO is added after stirring415g, control reaction temperature are equal to or less than 25 DEG C, stir 15min；By water-bath liter
Temperature continues stir about 1h to 30~40 DEG C；Stirring terminates the temperature of water-bath being warming up to 90 DEG C, by 300ml deionized water drop
Enter in solution；The H that 400ml mass concentration is 30% is measured simultaneously2O2, it is added in solution, solution becomes vivid from brownish black
Yellow；Continue to stir 10min, then solution is poured into beaker, 5~15min of ultrasound；Finally it is with the mass concentration of 1000ml
5.5% dilute hydrochloric acid filtering, is then sufficiently filtered until sulfate radical-free ion in filtrate with deionized water again.
Step 2.2, the resulting product of step 2.1 is dried using freeze drier, obtains spongy graphite oxide
Alkene；The graphene oxide of acquisition is put into airslide disintegrating mill again to crush, grinding time is 1~3 hour, obtains graphene oxide powder
Body.The partial size D90 of its graphene oxide powder obtained is less than 10 μm.
Step 3, graphene oxide powder made from step 2 is dissolved in deionized water, configuration concentration is the oxygen of 40mg/ml
Graphite alkene solution, and surfactant and alkaline reagent are added in proportion, solution is adjusted to neutral or alkalescent, then will
Its ultrasound 10min~30min, makes it be uniformly dispersed, obtains graphene oxide mixed solution.
Step 4, prepare that regenerated cellulose is compound to use cellulose pulp.
Weigh 500g regenerated cellulose compound pulp, by its be 35% according to mass ratio 1:3.5 and mass concentration hydrogen-oxygen
Change sodium solution mixing, blender stirs 20~50min, is thoroughly mixed it；Then it puts it into squeezer and squeezes, setting pressure
Power is 2~6kpa, and the squeezing time is 10~30min；Pulp is subjected to experienced processing again, experienced temperature is 20~25 DEG C, the time
For 3~5h, then temperature risen to 30~35 DEG C, continues aging, ageing time is 1~3h；It is carried out after the completion of experienced processing yellow
Change, 20~25 DEG C of yellow temperature, 20~30min of yellow time, then temperature is risen to 25~30 DEG C, continue yellow, the time is also
20~30min.
Step 5, graphene oxide mixed solution made from step 3 is warming up to 25~30 DEG C, then in proportion with step 4
Resulting pulp mixing, is stirred using blender, and the time is 20~50min, obtains regenerated cellulose composite fibre pulp, wherein
The ratio of graphene oxide solid content and pulp fibers element solid content is (0.01~5) %:1, obtains the compound fibre of regenerated cellulose
Tie up pulp.
Step 6, regenerated cellulose composite fibre pulp made from step 5 is subjected to spinning, prepares golden graphene oxide
Regenerated cellulose composite fibre.
Embodiment 5
A kind of gold graphene oxide regenerated cellulose composite fibre, raw material includes by mass percentage: regeneration is fine
Plain compound pulp 60% is tieed up, graphene oxide solution 10%, surfactant 5%, alkaline reagent 5%, surplus is water.
Preferably, surfactant is to include sodium lignin sulfonate, polyethylene pyrrole network alkanone (PVP), detergent alkylate sulphur
The mixture of sour sodium.
Sodium lignin sulfonate, polyethylene pyrrole network alkanone, neopelex mass ratio be 1:3:5.
Alkaline reagent includes ammonium hydroxide, and potassium hydroxide is any a variety of in sodium hydroxide.
The present embodiment additionally provides the preparation method of the gold graphene oxide regenerated cellulose composite fibre, it includes:
Step 1, each raw material is weighed in proportion.
Step 2, graphene oxide powder is prepared.
Preferably, graphene oxide is prepared using Hummers method, includes:
Step 2.1, into the 1000ml reaction flask being placed in water-bath be added 300ml mass concentration be 98% it is dense
H2SO4；Weigh 5g graphite powder and 2g NaNO respectively again3Solid, add it in reaction flask, turn on agitator stirring
30min；KMnO is added after stirring415g, control reaction temperature are equal to or less than 25 DEG C, stir 15min；By water-bath liter
Temperature continues stir about 1h to 30~40 DEG C；Stirring terminates the temperature of water-bath being warming up to 90 DEG C, by 300ml deionized water drop
Enter in solution；The H that 500ml mass concentration is 30% is measured simultaneously2O2, it is added in solution, solution becomes vivid from brownish black
Yellow；Continue to stir 10min, then solution is poured into beaker, 5~15min of ultrasound；Finally it is with the mass concentration of 1000ml
5.5% dilute hydrochloric acid filtering, is then sufficiently filtered until sulfate radical-free ion in filtrate with deionized water again.
Step 2.2, the resulting product of step 2.1 is dried using freeze drier, obtains spongy graphite oxide
Alkene；The graphene oxide of acquisition is put into airslide disintegrating mill again to crush, grinding time is 1~3 hour, obtains graphene oxide powder
Body.The partial size D90 of its graphene oxide powder obtained is less than 10 μm.
Step 3, graphene oxide powder made from step 2 is dissolved in deionized water, configuration concentration is the oxygen of 50mg/ml
Graphite alkene solution, and surfactant and alkaline reagent are added in proportion, solution is adjusted to neutral or alkalescent, then will
Its ultrasound 10min~30min, makes it be uniformly dispersed, obtains graphene oxide mixed solution.
Step 4, prepare that regenerated cellulose is compound to use cellulose pulp.
Weigh 500g regenerated cellulose compound pulp, by its be 40% according to mass ratio 1:4 and mass concentration hydroxide
Sodium solution mixing, blender stir 20~50min, are thoroughly mixed it；Then it puts it into squeezer and squeezes, set pressure
For 2~6kpa, the squeezing time is 10~30min；Pulp is subjected to experienced processing again, experienced temperature is 20~25 DEG C, the time 3
~5h, then temperature is risen to 30~35 DEG C, continue aging, ageing time is 1~3h；Yellow is carried out after the completion of experienced processing,
20~25 DEG C of yellow temperature, 20~30min of yellow time, then temperature is risen to 25~30 DEG C, continue yellow, the time is also 20~
30min。
Step 5, graphene oxide mixed solution made from step 3 is warming up to 25~30 DEG C, then in proportion with step 4
Resulting pulp mixing, is stirred using blender, and the time is 20~50min, obtains regenerated cellulose composite fibre pulp, wherein
The ratio of graphene oxide solid content and pulp fibers element solid content is (0.01~5) %:1, obtains the compound fibre of regenerated cellulose
Tie up pulp.
Step 6, regenerated cellulose composite fibre pulp made from step 5 is subjected to spinning, prepares golden graphene oxide
Regenerated cellulose composite fibre.
Gold graphene oxide regenerated cellulose composite fibre provided by the invention and preparation method thereof, newly draws in formula
Regenerated cellulose composite fibre is set to have the function of antibacterial, anti-mite, far infrared, uvioresistant etc. into a kind of graphene oxide.This hair
Graphene in bright uses graphene oxide, is then added to a kind of graphene oxide into regenerated cellulose composite fibre pulp
Solution, the solution contain certain density surfactant to realize the evenly dispersed of graphene oxide.The oxygen of this formula preparation
Graphite alkene is mainly used for, preparation golden graphene regenerated cellulose composite fibre compound with regenerated cellulose composite fibre.This
Invention can prepare the golden compound fibre of graphene regenerated cellulose with the functions such as antibacterial, anti-mite, uvioresistant, far infrared
Dimension promotes regenerated cellulose composite fibre added value, extends the use scope of regenerated cellulose composite fibre.
It is discussed in detail although the contents of the present invention have passed through above preferred embodiment, but it should be appreciated that above-mentioned
Description is not considered as limitation of the present invention.After those skilled in the art have read above content, for of the invention
A variety of modifications and substitutions all will be apparent.Therefore, protection scope of the present invention should be limited to the appended claims.
Claims (10)
1. a kind of gold graphene oxide regenerated cellulose composite fibre, which is characterized in that the raw material of the composite fibre is pressed
Mass percent meter includes: regenerated cellulose compound pulp 60%~84.9%, graphene oxide solution 0.1%~10%, table
Face activating agent 0.1%~5%, alkaline reagent 0.1%~5%, surplus are water.
2. gold graphene oxide regenerated cellulose composite fibre as described in claim 1, which is characterized in that the surface
Activating agent be comprising sodium lignin sulfonate, polyethylene pyrrole network alkanone, neopelex mixture.
3. gold graphene oxide regenerated cellulose composite fibre as claimed in claim 2, which is characterized in that the surface
Sodium lignin sulfonate in activating agent, polyethylene pyrrole network alkanone, neopelex mass ratio be 1:(1~3): (2~
5)。
4. gold graphene oxide regenerated cellulose composite fibre as described in claim 1, which is characterized in that the alkalinity
Reagent includes ammonium hydroxide, potassium hydroxide, any one or more in sodium hydroxide.
5. a kind of system of the golden graphene oxide regenerated cellulose composite fibre as described in any one of Claims 1 to 4
Preparation Method, which is characterized in that the method includes:
Step 1, each raw material is weighed in proportion；
Step 2, graphene oxide powder is prepared；
Step 3, graphene oxide powder made from step 2 is soluble in water, graphene oxide solution is configured, and it is living to add surface
Property agent and alkaline reagent, solution is adjusted to neutral or alkalescent makes it be uniformly dispersed then by its ultrasound, obtains oxidation stone
Black alkene mixed solution；
Step 4, regenerated cellulose compound pulp is weighed, it is mixed with sodium hydroxide solution, stirs, is thoroughly mixed it；So
After squeezed；Pulp is subjected to experienced processing again；Yellow is carried out after the completion of experienced processing；
Step 5, graphene oxide mixed solution made from step 3 is heated up, is then mixed with the resulting pulp of step 4, stirred,
Obtain regenerated cellulose composite fibre pulp；
Step 6, regenerated cellulose composite fibre pulp made from step 5 is subjected to spinning, prepares golden graphene oxide regeneration
Cellulose composite fiber.
6. the preparation method of gold graphene oxide regenerated cellulose composite fibre as claimed in claim 5, which is characterized in that
The step 2 includes:
Step 2.1, into the 1000ml reaction flask being placed in water-bath be added 100~300ml mass concentration be 98% it is dense
H2SO4；Weigh 5g graphite powder and 2g NaNO respectively again3Solid, add it in reaction flask, turn on agitator stirring
30min；KMnO is added after stirring415g, control reaction temperature are equal to or less than 25 DEG C, stir 15min；By water-bath liter
Temperature continues to stir 1h to 30~40 DEG C；Stirring terminates the temperature of water-bath being warming up to 90 DEG C, and 300ml deionized water is instilled
In solution；The H that 200~500ml mass concentration is 30% is measured simultaneously2O2, it is added in solution, solution becomes yellow from brownish black
Color；Continue to stir 10min, then solution is poured into beaker, 5~15min of ultrasound；Finally it is with the mass concentration of 1000ml
5.5% dilute hydrochloric acid filtering, is then sufficiently filtered until sulfate radical-free ion in filtrate with deionized water again；
Step 2.2, the resulting product of step 2.1 is dried using freeze drier, obtains spongy graphene oxide；Again
The graphene oxide of acquisition is put into airslide disintegrating mill to crush, grinding time is 1~3 hour, obtains graphene oxide powder.
7. the preparation method of gold graphene oxide regenerated cellulose composite fibre as claimed in claim 6, which is characterized in that
The partial size D90 of graphene oxide powder made from the step 2 is less than 10 μm.
8. the preparation method of gold graphene oxide regenerated cellulose composite fibre as claimed in claim 5, which is characterized in that
In the step 3, graphene oxide powder is dissolved in deionized water, configuration concentration is the graphene oxide of 1~50mg/ml
Solution, and surfactant and alkaline reagent are added in proportion, solution is adjusted to neutral or alkalescent, then by its ultrasound
10min~30min makes it be uniformly dispersed.
9. the preparation method of gold graphene oxide regenerated cellulose composite fibre as claimed in claim 5, which is characterized in that
In the step 4,500g regenerated cellulose compound pulp is weighed, by it according to mass ratio 1:(2~4) be with mass concentration
20%~40% sodium hydroxide solution mixing, blender stir 20~50min, are thoroughly mixed it；Then pressure is put it into
It is squeezed in crusher, sets pressure as 2~6kpa, the squeezing time is 10~30min；Pulp is subjected to experienced processing, experienced temperature again
Degree is 20~25 DEG C, and the time is 3~5h, then temperature is risen to 30~35 DEG C, continues aging, and ageing time is 1~3h；Experienced
Progress yellow after the completion of processing, 20~25 DEG C of yellow temperature, 20~30min of yellow time, then temperature is risen to 25~30 DEG C, after
Continuous yellow, the time is also 20~30min.
10. the preparation method of gold graphene oxide regenerated cellulose composite fibre as claimed in claim 5, feature exist
In, in the step 5, graphene oxide mixed solution is warming up to 25~30 DEG C, is then mixed in proportion with pulp, use
Blender stirring, the time be 20~50min, obtain regenerated cellulose composite fibre pulp, wherein graphene oxide solid content with
The ratio of pulp fibers element solid content is (0.01~5) %:1.
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| CN114031808A (en) * | 2021-12-13 | 2022-02-11 | 罗莱生活科技股份有限公司 | Regenerated cellulose fiber/aerogel composite material and preparation method thereof |
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Application publication date: 20190827 |