CN109913965A - A kind of alkali systems primary reconstruction cellulose/graphene composite fibre and preparation method thereof altogether - Google Patents
A kind of alkali systems primary reconstruction cellulose/graphene composite fibre and preparation method thereof altogether Download PDFInfo
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Abstract
The present invention relates to a kind of alkali systems primary reconstruction cellulose/graphene fiber materials and preparation method thereof altogether, are made of graphene dispersing solution and cellulose solution, and the solvent of cellulose solution is made of highly basic composition, urea or thiocarbamide and water.Preparation process mainly includes intercalation, activation, and shearing removing, aqueous slkali dispersion, obtains the graphene dispersing solution of high concentration altogether；The dissolution of cellulose is cooled to -12 DEG C--4 DEG C firstly the need of that will be total to alkali soluble agent, and high-speed stirred quickly dissolves molecular weight less than 10 × 104Natural or regenerated cellulose, obtain the transparency cellulose concentrated solution of high-dissolvability.After cellulose solution under alkali systems is mixed with graphene dispersing solution with appropriate proportioning solution, the diluted acid coagulating bath self assembly through 3-5 wt%, drawing-off oils, and cellulose/graphene fiber material is prepared in drying.Operation of the present invention is simple, and prepared material can be used for dressing the fields such as self power generation smart fabric, antistatic textile material, flexible intelligent sensing material or Electromagnetically shielding fabrics.
Description
Technical field
The present invention relates to a kind of alkali systems primary reconstruction cellulose/graphene composite fibres and preparation method thereof altogether, belong to
In chemistry and materialogy field, further subdivision belongs to functional composite material preparation and application field.
Background technique
Intelligence is the important directions of the following fibrous material development, and electronic technology is merged and is sensed, electromagnetic shielding, joule adds
Heat, communication, the technologies such as artificial intelligence, which further integrate tencel, can greatly improve the functionality of fiber, expand it in intelligence
The application in the wearable field of energy, and the basic premise for obtaining use above is to prepare conductive fiber.For flexible wearable with leading
The preparation of electric fiber, existing technology mostly use conductive filler (conductive black, carbon nanotube or graphene) and fibrous material into
Row physical blending coats conductive coating in fibrous material surface to realize.It can be seen that conductive material and fibrous matrix
Selection be conductive fiber preparation important composition.Cellulose is a kind of natural reproducible high molecular material, makes full use of fiber
Element not only can protect environment, but also can save limited petroleum resources.Regenerated celulose fibre has similar to cotton fiber
Clothes performance, while grafting and functional treatment can be carried out by the chemical reaction of hydroxyl in its macromolecular, therefore it can make
For the matrix of functional fibre.Graphene is a kind of two-dimentional carbon material being concerned in recent years, since itself has stable be total to
Yoke electron system, thus show the excellent physical properties such as many mechanical properties, electrical and thermal conductivity performance, chemical stability.
By graphene with cellulose in-situ is compound prepares conductive fiber, can integrate cellulose fibre can braided nature and graphene
Highly conductive characteristic, and then realize the flexible wearable of intelligent fiber.However, dissolution or the grapheme material of either cellulose
Preparation and stable dispersion, be the problem that field of scientific study is generally accepted.
103046151 B of patent CN is mixed using graphene oxide dispersion with regenerated cellulose solution, wet by viscose glue
After the molding of method spinning technique, then through reduction regenerated cellulose/graphene composite fibre is prepared, although fibrous material is in mechanical strength
Aspect is promoted (its dry breaking strength is up to 2 .62cN/dtex, and wet breaking strength reaches 1 .54cN/dtex), but
It is that graphene oxide in system can not be restored thoroughly and cause the electric conductivity of fiber not high.104328523 B of patent CN passes through life
It is mixed that substance graphene aqueous dispersions or other solvent graphene dispersing solutions (108411395 A of CN) and cellulose carry out solution
It closes further wet spinning and obtains filled-type graphene/regenerated celulose fibre, however graphene in aqueous solution bad point
Dissipating causes graphene in fiber system to be reunited seriously, and in order to solve that graphite can be brought after surfactant is added in agglomeration traits
Alkene electric conductivity is greatly lowered, and then leads to the implementation of the program there are some problems.In addition to composite spinning, to existing
It is also the important channel (108774879 A of CN) for obtaining conductive fiber that fibrous material, which carries out surface coating, however either
By still utilizing electrostatic adsorption to combine more coating materials to Fiber strength, fiber is by using or washing
Afterwards, conductive coating can tail off or disappear, and then electric conductivity is significantly deteriorated.
Up to now, it using the graphene of high quality and cellulose as raw material, is mixed by in-situ solution, self assembly Wet-spinning
Silk technology preparation has superior electrical conductivity energy, high-intensitive, can weave, the functional graphene/cellulose being produced on a large scale is multiple
Condensating fiber material is still a difficult point of ongoing research area.
Summary of the invention
Present invention seek to address that the bad caused filamentary conductive of graphene dispersion in existing cellulose/graphene fiber
The not high problem with mechanical strength, to obtain the conductive characteristic of the fibrous material, strength characteristics and can braided nature association
With improving, the fibrous material is further applied to wearable self power generation smart fabric, antistatic textile material, flexible intelligent
Sensing material, the fields such as Electromagnetically shielding fabrics and Joule heating function fabric.For this purpose, the purpose of the present invention is to provide one kind
Alkali systems primary reconstruction cellulose/graphene composite fibre and preparation method thereof altogether.
A kind of alkali systems primary reconstruction cellulose/graphene fiber material altogether proposed by the present invention, the total alkali body
It is that primary reconstruction cellulose/graphene fiber material is made of cellulose solution and graphene dispersing solution, in which: the fibre
Tieing up the solvent group in plain solution becomes the alkali compounds of 3-10wt%, and the urea or thiocarbamide of 3-20wt%, remaining is water, gross weight
Amount meets 100%；The mass ratio of cellulose solution and graphene dispersing solution is 100:1-1:1.
In the present invention, in the solvent of the cellulose solution, alkali compounds includes sodium hydroxide, potassium hydroxide, hydrogen-oxygen
Change lithium, sodium carbonate, potassium carbonate, lithium carbonate, sodium bicarbonate, saleratus, lithium bicarbonate, ammonium hydroxide or tetrabutylammonium
One of or any combination between them.
In the present invention, the content of cellulose in the cellulose solution is 0.2-20 wt%.
In the present invention, the cellulose is molecular weight less than 10 × 104Natural or regenerated cellulose.
The preparation method of alkali systems primary reconstruction cellulose/graphene fiber material altogether proposed by the present invention is specific to walk
It is rapid as follows:
(1) preparation of graphene dispersing solution
It is then directly water-soluble in alkalinity to reduce its Interaction between layers using intercalator to graphite intercalation using graphite as raw material
Ultrasound is carried out to intercalated graphite in liquid or shearing is removed, altogether aqueous slkali dispersion, and then obtains the graphene dispersion of high degree of dispersion
Liquid；
(2) preparation of cellulose solution
By alkali compounds, urea or thiocarbamide and water are uniformly mixed, and the solvent of cellulose solution are obtained, by cellulose solution
Solvent is cooled to -12 DEG C--4 DEG C, and cellulose is added in the solvent of cellulose solution, high-speed stirred, keeps cellulose instant fastly
Solution, obtains the transparency cellulose concentrated solution of high-dissolvability；
(3) after mixing the cellulose solution that step (2) obtains in proportion with the graphene dispersing solution that step (1) obtains, through 3-
The diluted acid coagulating bath self assembly of 5wt%, drawing-off oil, dry, and cellulose/graphene fiber material is prepared.
Compared with prior art, the invention has the advantages that and effect:
Preparation process is simple, at low cost.Alkali soluble agent composition is the cheap raw material of industry, the dissolution of cellulose altogether selected by the present invention
The feasibility of large-scale production is provided with the preparation method of graphene；
Cellulose makes full use of cellulose not only to can protect environment as a kind of natural renewable polymeric materials, but also
Limited petroleum resources can be saved.Cellulose itself has good mechanical property, moisture pick-up properties, but does not have conduction
Property, traditional scheme is by the way that conducting polymer or conductive filler is added to prepare conductive cellulose fiber, but conductive component
The mechanical mechanics property that often will affect cellulose fibre is added, while conductivity is lower.The graphite removed in total alkali soluble agent
Alkene and cellulose molecular chain form stable dispersion by interaction of hydrogen bond, with traditional physical blending graphene/
Cellulose strategy compares, and the present invention realizes molecularly dispersed structure truly.It is self-assembly of in diluted acid coagulating bath
Composite fibre realizes the orientation of cellulose molecular chain and aligning for graphene film after drawing-off, and then effectively improves
The Mechanics of Machinery intensity of composite fibre is prepared, while compared with common preparation method, graphene aligned more easily
Good conductive path is formed, and then obtains the conductive fiber of macroscopic view.
Other features and advantages of the present invention will be explained in the following detailed description section.
Detailed description of the invention
The drawings are intended to provide a further understanding of the invention, and constitutes part of specification, with following reality
It applies mode to be used to explain the present invention together, but is not construed as limiting the invention.In the accompanying drawings:
Fig. 1 shows cellulose solution prepared in accordance with the present invention, cellulose/graphene composite spinning precursor solution.
Fig. 2 shows the cellulose in the present invention, graphene, regenerated celulose fibre, celluloses/graphene composite fibre
XRD diagram.
It is compound that Fig. 3 shows the cellulose in the present invention/graphene composite fibre electron scanning micrograph (a)
The surface topography of fiber, (b) composite fiber surface pattern enlarged drawing；(c) cross-section morphology of composite fibre；(d) is compound
The cross-section morphology enlarged drawing of fiber.
Fig. 4 shows the digital camera photo of (a) in present invention cellulose/graphene fiber, and (b) optical microscopy shines
Piece, (c) single fiber can bear a heavy burden 10 grams of counterweight digital camera photo.
Specific embodiment
Below in conjunction with attached drawing, specific embodiments of the present invention will be described in detail.It should be understood that this place
The specific embodiment of description is merely to illustrate and explain the present invention, and is not intended to restrict the invention.
Embodiment 1
By 4 parts of celluloses, (molecular weight is 8 × 104) be dissolved in 100 parts of basic solvents, solvent group become 8 wt%NaOH, 12
Wt% urea is divided into water with group.After total alkali soluble agent is cooled to -12 DEG C first, then cooling solvent high speed stirring quickly dissolution
Cellulose obtains transparency cellulose solution.After crystalline flake graphite is activated by sulfuric acid intercalation, intercalated graphite is cleaned to neutrality,
Ultrasound removing 2 hours, cut at a high speed after cellulose solution is mixed with graphene dispersing solution in the sodium hydrate aqueous solution of PH=14
Cutting dissipates (cellulose and graphene mass ratio 10:1 in solution), further by the above cellulose/graphene spinning forerunner
Sulfuric acid of the liquid solution through 5 wt%/10 wt% aqueous sodium persulfate solution coagulating baths carry out fiber self assembly, and further drawing-off oils, and do
Regenerated cellulose/graphene complex fiber material is prepared after dry.Graphene forms good in strong base solution in the present embodiment
Good removing disperses solution, and the presence in precursor solution between cellulose and graphene due to hydrogen bond action forms molecular level
It is mixed to form two-arch tunnel, and then the fiber prepared by wet spinning is made to be provided with the electric conductivity of up to 1.2 S/m, while material
Material maintains good intensity and toughness.
Embodiment 2
By 8 parts of celluloses, (molecular weight is 5 × 104) be dissolved in 100 parts of basic solvents, solvent group become 10 wt%LiOH, 12
Wt% thiocarbamide is divided into water with group.After total alkali soluble agent is cooled to -10 DEG C first, then cooling solvent high speed stirring quickly dissolution
Cellulose obtains transparency cellulose solution.After crystalline flake graphite is activated by sulfuric acid intercalation, intercalated graphite is cleaned to neutrality,
Ultrasound removing 2 hours, cut at a high speed after cellulose solution is mixed with graphene dispersing solution in the lithium hydroxide aqueous solution of PH=14
Cutting dissipates (cellulose and graphene mass ratio 20:1 in solution), further by the above cellulose/graphene spinning forerunner
Hydrochloric acid of the liquid solution through 10wt%/15 wt% sodium-chloride water solution coagulating baths carry out fiber self assembly, and further drawing-off oils, and do
Regenerated cellulose/graphene complex fiber material is prepared after dry.Graphene forms good in strong base solution in the present embodiment
Good removing disperses solution, and the presence in precursor solution between cellulose and graphene due to hydrogen bond action forms molecular level
It is mixed to form two-arch tunnel, and then the fiber prepared by wet spinning is made to be provided with the electric conductivity of up to 0.9 S/m, while material
Material maintains good intensity and toughness.
Embodiment 3
By 6 parts of celluloses, (molecular weight is 4 × 104) be dissolved in 100 parts of basic solvents, solvent group become 6 wt%NaOH, 8
Wt% thiocarbamide is divided into water with group.After total alkali soluble agent is cooled to -10 DEG C first, then cooling solvent high speed stirring quickly dissolution
Cellulose obtains transparency cellulose solution.After crystalline flake graphite is activated by sulfuric acid intercalation, intercalated graphite is cleaned to neutrality,
Ultrasound removing 2 hours, cellulose solution and graphene dispersing solution are mixed in sodium hydroxide/thiocarbamide mixed aqueous solution of PH=12
High speed shear dispersion (cellulose and graphene mass ratio 8:1 in solution) after conjunction, further by above cellulose/graphene
Spinning precursor solution carries out fiber self assembly through phytic acid aqueous coagulation bath, and further drawing-off oils, and prepares again after dry
Raw cellulose/graphene complex fiber material.Graphene forms good removing dispersion in strong base solution in the present embodiment
Solution, the presence in precursor solution between cellulose and graphene due to hydrogen bond action form molecular level and are mixed to form doubly-linked
Continuous phase, and then the fiber prepared by wet spinning is made to be provided with the electric conductivity of up to 2.16 S/m, at the same material maintain it is good
Good intensity and toughness.
Comparative example 1
By 5 parts of celluloses, (molecular weight is 5 × 104) be dissolved in 100 parts of basic solvents, solvent group become 5 wt%NaOH, 10
Wt% urea is divided into water with group, 3 parts of conductive blacks will be directly added into mixed solution after cellulose dissolution in low temperature, machinery stirs
After mixing 5 hours, spinning is carried out with cellulose mixture/conductive black spinning solution, using the aqueous sulfuric acid of 10 wt% concentration as coagulating
Gu bath, by drawing-off, oils, cellulose/conductive black composite fibre is obtained after dry.Carbon black is in aqueous solution in the present embodiment
And not formed good dispersion, by reuniting, shark leather jacket microprotrusion knot is presented in the fiber for seriously institute's wet spinning being caused to prepare
Structure, while the electric conductivity of fiber only has 0.08 S/m, tenacity of fibre is bad.
It is noted that the above content is combine specific preferred embodiment made for the present invention further specifically
It is bright, and it cannot be said that a specific embodiment of the invention is only limitted to this, for the ordinary skill people of the technical field of the invention
For member, under the premise of not departing from design of the invention, several simple deductions or replacement can also be made, should all be regarded
Scope of patent protection is determined to belong to claims that the present invention is submitted.
Claims (5)
1. a kind of alkali systems primary reconstruction cellulose/graphene fiber material altogether, which is characterized in that the total alkali systems are former
Position self assembly cellulose/graphene fiber material is made of cellulose solution and graphene dispersing solution, in which: the cellulose
Solvent group in solution becomes the alkali compounds of 3-10wt%, and the urea or thiocarbamide of 3-20wt%, remaining is water, and total weight is full
Foot 100%；The mass ratio of cellulose solution and graphene dispersing solution is 100:1-1:1.
2. alkali systems primary reconstruction cellulose/graphene fiber material altogether according to claim 1, which is characterized in that
In the solvent of the cellulose solution, alkali compounds includes sodium hydroxide, potassium hydroxide, lithium hydroxide, sodium carbonate, carbonic acid
One of potassium, lithium carbonate, sodium bicarbonate, saleratus, lithium bicarbonate, ammonium hydroxide or tetrabutylammonium or they it
Between any combination.
3. alkali systems primary reconstruction cellulose/graphene fiber material altogether according to claim 1, which is characterized in that
Content of cellulose in the cellulose solution is 0.2-20 wt%.
4. alkali systems primary reconstruction cellulose/graphene fiber material altogether according to claim 1, which is characterized in that
The cellulose is molecular weight less than 10 × 104Natural or regenerated cellulose.
5. a kind of be total to alkali systems primary reconstruction cellulose/graphene fiber material preparation method as described in claim 1,
It is characterized in that, specific step is as follows:
(1) preparation of graphene dispersing solution
It is then directly water-soluble in alkalinity to reduce its Interaction between layers using intercalator to graphite intercalation using graphite as raw material
Ultrasound is carried out to intercalated graphite in liquid or shearing is removed, altogether aqueous slkali dispersion, and then obtains the graphene dispersing solution of high concentration；
(2) preparation of cellulose solution
By alkali compounds, urea or thiocarbamide and water are uniformly mixed, and the solvent of cellulose solution are obtained, by cellulose solution
Solvent is cooled to -12 DEG C--4 DEG C, and cellulose is added in the solvent of cellulose solution, high-speed stirred, keeps cellulose instant fastly
Solution, obtains the transparency cellulose concentrated solution of high-dissolvability；
(3) after mixing the cellulose solution that step (2) obtains in proportion with the graphene dispersing solution that step (1) obtains, through 3-
The diluted acid coagulating bath self assembly of 5wt%, drawing-off oil, dry, and cellulose/graphene fiber material is prepared.
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| CN113862992A (en) * | 2021-09-10 | 2021-12-31 | 东南大学 | Sodium alginate-based composite electricity generating fiber and preparation method thereof |
| CN114507910A (en) * | 2022-02-22 | 2022-05-17 | 西安工程大学 | Nano-aramid fiber reinforced regenerated cellulose fiber material, preparation method and application |
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