CN109913965B - In-situ self-assembly cellulose/graphene composite fiber of co-alkali system and preparation method thereof - Google Patents
In-situ self-assembly cellulose/graphene composite fiber of co-alkali system and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a co-alkali system in-situ self-assembly cellulose/graphene fiber material and a preparation method thereof. The preparation process mainly comprises intercalation, activation, shearing and stripping, and dispersion of a co-alkali solution to obtain a high-concentration graphene dispersion solution; the dissolution of cellulose firstly needs to cool the co-alkali solvent to-12 ℃ to-4 ℃, and the molecular weight is rapidly dissolved to be less than 10 multiplied by 10 by stirring at high speed4To obtain a transparent cellulose concentrated solution with high solubility. Mixing a cellulose solution in an alkali system with a graphene dispersion solution according to a proper proportion, carrying out self-assembly by a 3-5wt% diluted acid coagulating bath, drafting, oiling, and drying to prepare the cellulose/graphene fiber material. The method is simple to operate, and the prepared material can be used in the fields of wearable self-generating intelligent fabrics, antistatic textile materials, flexible intelligent sensing materials or electromagnetic shielding fabrics and the like.
Description
Technical Field
The invention relates to a co-alkali system in-situ self-assembly cellulose/graphene composite fiber and a preparation method thereof, belongs to the fields of chemistry and materials science, and further belongs to the fields of preparation and application of functional composite materials.
Background
The intellectualization is an important direction for the development of future fiber materials, the electronic technology is integrated with the sensing, electromagnetic shielding, Joule heating, communication, artificial intelligence and other technologies, the novel fiber can be further integrated, the functionality of the fiber can be greatly improved, the application of the novel fiber in the intelligent wearable field is expanded, and the basic premise for obtaining the application is to prepare the conductive fiber. For the preparation of the flexible wearable conductive fiber, the existing technology is mostly realized by physically blending a conductive filler (conductive carbon black, carbon nanotube or graphene) and a fiber material or coating a conductive coating on the surface of the fiber material. It follows that the choice of conductive material and fiber matrix is an important component of the conductive fiber preparation. Cellulose is a natural renewable polymer material, and the cellulose is fully utilized, so that the environment can be protected, and limited petroleum resources can be saved. The regenerated cellulose fiber has the garment performance similar to that of cotton fiber, and can be used as the matrix of functional fiber through grafting and functional finishing by the chemical reaction of hydroxyl on macromolecules. Graphene is a two-dimensional carbon material which has attracted much attention in recent years, and exhibits many excellent physical properties such as mechanical properties, electrical and thermal conductivity, and chemical stability due to its own stable conjugated electron system. Graphene and cellulose are compounded in situ to prepare the conductive fibers, so that the weaving characteristic of the cellulose fibers and the high-conductivity characteristic of the graphene can be integrated, and the flexible and wearable intelligent fibers are further realized. However, dissolution of cellulose or preparation and stable dispersion of graphene materials are generally recognized problems in the field of scientific research.
Patent CN 103046151B utilizes graphene oxide dispersion liquid to mix with regenerated cellulose solution, and after forming through viscose wet spinning process, the regenerated cellulose/graphene composite fiber is prepared by reduction, although the mechanical strength of the fiber material is improved (its dry breaking strength is up to 2.62 CN/dtex, wet breaking strength is up to 1.54 CN/dtex), graphene oxide in the system can not be reduced completely, resulting in low conductivity of the fiber. In patent CN 104328523B, a biomass graphene aqueous dispersion or other solvent graphene dispersion (CN 108411395 a) and cellulose are subjected to solution mixing and further wet spinning to obtain filled graphene/regenerated cellulose fibers, however, poor dispersion of graphene in an aqueous solution leads to serious graphene aggregation in a fiber system, and a surfactant is added to solve the aggregation problem, which leads to a substantial decrease in graphene conductivity, and further leads to a certain problem in implementation of the scheme. Besides blend composite spinning, surface coating of the existing fiber material is also an important way to obtain the conductive fiber (CN 108774879 a), however, no matter by surface treatment or by combining more coating materials by electrostatic adsorption, the conductive coating is reduced or eliminated after the fiber is used or washed, and the conductivity is significantly deteriorated.
At present, a functional graphene/cellulose composite fiber material which has excellent conductivity, high strength, spinnability and large-scale production and is prepared by taking high-quality graphene and cellulose as raw materials through in-situ solution mixing and a self-assembly wet spinning technology is still a difficulty in the current research field.
Disclosure of Invention
The invention aims to solve the problem of low fiber conductivity and mechanical strength caused by poor dispersion of graphene in the existing cellulose/graphene fiber, so as to obtain the synergistic improvement of the conductivity, strength and weaving characteristics of the fiber material, and further apply the fiber material to the fields of wearable self-generating intelligent fabrics, antistatic textile materials, flexible intelligent sensing materials, electromagnetic shielding fabrics, Joule heating functional fabrics and the like. Therefore, the invention aims to provide the cellulose/graphene composite fiber in-situ self-assembled by the co-alkali system and the preparation method thereof.
The invention provides an in-situ self-assembly cellulose/graphene fiber material of a co-alkali system, which consists of a cellulose solution and a graphene dispersion solution, wherein: the solvent in the cellulose solution comprises 3-10wt% of alkaline compound, 3-20wt% of urea or thiourea and the balance of water, and the total weight of the solvent is 100%; the mass ratio of the cellulose solution to the graphene dispersion liquid is 100:1-1: 1.
In the present invention, in the solvent of the cellulose solution, the basic compound includes one of sodium hydroxide, potassium hydroxide, lithium hydroxide, sodium carbonate, potassium carbonate, lithium carbonate, sodium bicarbonate, potassium bicarbonate, lithium bicarbonate, ammonium hydroxide, or tetrabutylammonium hydroxide, or any combination thereof.
In the invention, the cellulose content in the cellulose solution is 0.2-20 wt%.
In the invention, the cellulose has a molecular weight of less than 10 x 104Natural or regenerated cellulose.
The invention provides a preparation method of a co-alkali system in-situ self-assembled cellulose/graphene fiber material, which comprises the following specific steps:
(1) preparation of graphene dispersion
The method comprises the following steps of (1) intercalating graphite by using an intercalating agent to reduce the interaction between layers of the graphite by using the graphite as a raw material, then directly carrying out ultrasonic or shear stripping on the intercalated graphite in an alkaline aqueous solution, and dispersing with a co-alkali solution to obtain a highly dispersed graphene dispersion solution;
(2) preparation of cellulose solution
Uniformly mixing an alkaline compound, urea or thiourea and water to obtain a solvent of a cellulose solution, cooling the solvent of the cellulose solution to-12-4 ℃, adding cellulose into the solvent of the cellulose solution, and stirring at a high speed to rapidly dissolve the cellulose to obtain a high-solubility transparent cellulose concentrated solution;
(3) and (3) mixing the cellulose solution obtained in the step (2) and the graphene dispersion liquid obtained in the step (1) in proportion, and then carrying out self-assembly, drafting, oiling and drying on the mixture by using 3-5wt% of dilute acid coagulation bath to prepare the cellulose/graphene fiber material.
Compared with the prior art, the invention has the following advantages and effects:
the preparation process is simple and the cost is low. The components of the selected co-alkali solvent are all cheap industrial raw materials, and the cellulose dissolution and the graphene preparation scheme have feasibility of large-scale production;
cellulose is used as a natural renewable polymer material, and the cellulose is fully utilized, so that the environment can be protected, and limited petroleum resources can be saved. Cellulose has good mechanical property and moisture absorption performance, but does not have conductivity, and the traditional scheme is to prepare conductive cellulose fibers by adding conductive polymers or conductive fillers, but the mechanical property of the cellulose fibers is affected by the addition of conductive components, and the conductivity is low. Compared with the traditional physical blending graphene/cellulose strategy, the method realizes the molecular level dispersion in the real sense. The composite fiber formed by self-assembly in the dilute acid coagulation bath realizes the orientation of cellulose molecular chains and the directional arrangement of graphene sheets after drafting, so that the mechanical strength of the prepared composite fiber is effectively improved, and simultaneously, compared with a common preparation method, the directional arrangement of graphene is easier to form a good conductive path, so that macroscopic conductive fiber is obtained.
Additional features and advantages of the invention will be set forth in the detailed description which follows.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the principles of the invention without limiting the invention. In the drawings:
fig. 1 shows a cellulose solution, a cellulose/graphene composite spinning precursor solution, prepared according to the present invention.
Fig. 2 shows XRD patterns of cellulose, graphene, regenerated cellulose fiber, and cellulose/graphene composite fiber in the present invention.
Fig. 3 shows a scanning electron microscope photograph of a cellulose/graphene composite fiber according to the present invention (a) showing a surface topography of the composite fiber, and (b) showing an enlarged view of the surface topography of the composite fiber; (c) the profile morphology of the composite fiber; (d) an enlarged view of the profile of the composite fiber.
Fig. 4 shows (a) a digital camera photograph of cellulose/graphene fibers, (b) an optical microscope photograph, and (c) a digital camera photograph of a weight that can be loaded with 10 grams of a single fiber in the present invention.
Detailed Description
The following detailed description of embodiments of the invention refers to the accompanying drawings. It should be understood that the detailed description and specific examples, while indicating the present invention, are given by way of illustration and explanation only, not limitation.
Example 1
4 parts of cellulose (molecular weight 8X 10)4) Dissolved in 100 parts of alkaline solvent, the solvent composition is 8 wt% NaOH, 12 wt% urea, and the other component is water. Firstly, cooling the co-alkali solvent to-12 ℃, then cooling the solvent, and rapidly stirring and dissolving the cellulose at high speed to obtain a transparent cellulose solution. After the flake graphite is activated by sulfuric acid intercalation, cleaning the intercalated graphite to be neutral, ultrasonically stripping the flake graphite in a sodium hydroxide aqueous solution with the pH =14 for 2 hours, mixing a cellulose solution with a graphene dispersion solution, then shearing and dispersing the mixture at a high speed (the mass ratio of the cellulose to the graphene in the solution is 10: 1), further carrying out fiber self-assembly on the cellulose/graphene spinning precursor solution by a coagulating bath of 5wt% sulfuric acid/10 wt% sodium sulfate aqueous solution, further drafting, oiling, and drying to prepare the regenerated cellulose/graphene composite fiber material. In the embodiment, graphene forms a good stripping dispersion solution in a strong alkali solution, and cellulose and graphene in a precursor solution form molecular mixing to form a bicontinuous phase due to the existence of hydrogen bond, so that the fiber prepared by wet spinning has conductivity as high as 1.2S/m, and meanwhile, the material maintains good strength and toughness.
Example 2
8 parts of cellulose (molecular weight is 5 multiplied by 10)4) Dissolved in 100 parts of an alkaline solvent having a composition of 10% by weight of LiOH, 12% by weight of thiourea and a composition of water. Firstly, cooling the co-alkali solvent to-10 ℃, then cooling the solvent, and rapidly stirring and dissolving the cellulose at high speed to obtain a transparent cellulose solution. After flake graphite is intercalated and activated by sulfuric acid, the intercalated graphite is cleaned to be neutral, ultrasonic stripping is carried out for 2 hours in lithium hydroxide aqueous solution with PH =14, cellulose solution and graphene dispersion liquid are mixed and then are sheared at high speedDispersing (the mass ratio of cellulose to graphene in the solution is 20: 1), further performing fiber self-assembly on the cellulose/graphene spinning precursor solution through a coagulating bath of 10wt% hydrochloric acid/15 wt% sodium chloride aqueous solution, further drafting, oiling, and drying to prepare the regenerated cellulose/graphene composite fiber material. In the embodiment, graphene forms a good stripping dispersion solution in a strong alkali solution, and cellulose and graphene in a precursor solution form molecular mixing to form a bicontinuous phase due to the existence of hydrogen bond, so that the fiber prepared by wet spinning has conductivity as high as 0.9S/m, and meanwhile, the material maintains good strength and toughness.
Example 3
6 parts of cellulose (molecular weight 4X 10)4) Dissolved in 100 parts of alkaline solvent, the solvent composition is 6 wt% NaOH, 8 wt% thiourea, and the component is water. Firstly, cooling the co-alkali solvent to-10 ℃, then cooling the solvent, and rapidly stirring and dissolving the cellulose at high speed to obtain a transparent cellulose solution. After the flake graphite is intercalated and activated by sulfuric acid, cleaning the intercalated graphite to be neutral, ultrasonically stripping the flake graphite in a sodium hydroxide/thiourea mixed aqueous solution with the pH =12 for 2 hours, mixing a cellulose solution with a graphene dispersion solution, shearing and dispersing the mixture at a high speed (the mass ratio of the cellulose to the graphene in the solution is 8: 1), further carrying out fiber self-assembly on the cellulose/graphene spinning precursor solution through a phytic acid aqueous solution coagulating bath, further drafting, oiling, and drying to prepare the regenerated cellulose/graphene composite fiber material. In the embodiment, graphene forms a good stripping dispersion solution in a strong alkali solution, and cellulose and graphene in a precursor solution form molecular mixing to form a bicontinuous phase due to the existence of hydrogen bond, so that the fiber prepared by wet spinning has conductivity as high as 2.16S/m, and meanwhile, the material maintains good strength and toughness.
Comparative example 1
5 parts of cellulose (molecular weight is 5 multiplied by 10)4) Dissolving in 100 parts of alkaline solvent, wherein the solvent comprises 5wt% of NaOH and 10wt% of urea, and the solvent and the component are water, dissolving cellulose at low temperature, and directly adding 3 parts of conductive carbon blackAnd mechanically stirring the mixed solution for 5 hours, spinning by using the mixed cellulose/conductive carbon black spinning solution, taking a 10wt% sulfuric acid aqueous solution as a coagulating bath, and obtaining the cellulose/conductive carbon black composite fiber after drafting, oiling and drying. In the embodiment, the carbon black does not form good dispersion in an aqueous solution, the fiber prepared by wet spinning has a shark skin-mounted micro-protrusion structure due to serious agglomeration, the electrical conductivity of the fiber is only 0.08S/m, and the toughness of the fiber is poor.
It should be noted that the above-mentioned description is given for illustrating the present invention in more detail with reference to specific preferred embodiments, and it should not be considered that the present invention is limited to the specific embodiments, but rather that several simple deductions or substitutions can be made by those skilled in the art without departing from the spirit of the present invention, which should be regarded as belonging to the patent protection scope defined by the claims filed with the present invention.
Claims (5)
1. The in-situ self-assembly cellulose/graphene fiber material of the co-alkali system is characterized in that the raw material of the in-situ self-assembly cellulose/graphene fiber material of the co-alkali system consists of a cellulose solution and a graphene dispersion solution, wherein: the solvent in the cellulose solution comprises 3-10wt% of alkaline compound, 3-20wt% of urea or thiourea and the balance of water, and the total weight of the solvent is 100%; the mass ratio of the cellulose solution to the graphene dispersion liquid is 100:1-1: 1;
the preparation method of the co-alkali system in-situ self-assembled cellulose/graphene fiber material comprises the following specific steps:
(1) preparation of graphene dispersion
The method comprises the following steps of (1) intercalating graphite by using an intercalating agent to reduce the interaction between layers of the graphite by using the graphite as a raw material, then directly carrying out ultrasonic or shear stripping on the intercalated graphite in an alkaline aqueous solution, and dispersing with a co-alkali solution to obtain a high-concentration graphene dispersion solution;
(2) preparation of cellulose solution
Uniformly mixing an alkaline compound, urea or thiourea and water to obtain a solvent of a cellulose solution, cooling the solvent of the cellulose solution to-12-4 ℃, adding cellulose into the solvent of the cellulose solution, and stirring at a high speed to rapidly dissolve the cellulose to obtain a high-solubility transparent cellulose concentrated solution;
(3) and (3) mixing the cellulose solution obtained in the step (2) and the graphene dispersion liquid obtained in the step (1) in proportion, and then carrying out self-assembly, drafting, oiling and drying on the mixture by using 3-5wt% of dilute acid coagulation bath to prepare the cellulose/graphene fiber material.
2. The co-alkali system in-situ self-assembled cellulose/graphene fiber material according to claim 1, wherein in the solvent of the cellulose solution, the alkali compound comprises one of sodium hydroxide, potassium hydroxide, lithium hydroxide, sodium carbonate, potassium carbonate, lithium carbonate, sodium bicarbonate, potassium bicarbonate, lithium bicarbonate, ammonium hydroxide or tetrabutylammonium hydroxide or any combination thereof.
3. The co-alkali system in-situ self-assembled cellulose/graphene fiber material according to claim 1, wherein the cellulose content in the cellulose solution is 0.2-20 wt%.
4. The co-alkali system in-situ self-assembled cellulose/graphene fiber material according to claim 1, wherein the cellulose is a cellulose with a molecular weight of less than 10 x 104Natural or regenerated cellulose.
5. The preparation method of the co-alkali system in-situ self-assembled cellulose/graphene fiber material according to claim 1 is characterized by comprising the following specific steps:
(1) preparation of graphene dispersion
The method comprises the following steps of (1) intercalating graphite by using an intercalating agent to reduce the interaction between layers of the graphite by using the graphite as a raw material, then directly carrying out ultrasonic or shear stripping on the intercalated graphite in an alkaline aqueous solution, and dispersing with a co-alkali solution to obtain a high-concentration graphene dispersion solution;
(2) preparation of cellulose solution
Uniformly mixing an alkaline compound, urea or thiourea and water to obtain a solvent of a cellulose solution, cooling the solvent of the cellulose solution to-12-4 ℃, adding cellulose into the solvent of the cellulose solution, and stirring at a high speed to rapidly dissolve the cellulose to obtain a high-solubility transparent cellulose concentrated solution;
(3) and (3) mixing the cellulose solution obtained in the step (2) and the graphene dispersion liquid obtained in the step (1) in proportion, and then carrying out self-assembly, drafting, oiling and drying on the mixture by using 3-5wt% of dilute acid coagulation bath to prepare the cellulose/graphene fiber material.
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