CN112877908A - Light high-strength multilayer nanofiber composite material and preparation method thereof - Google Patents
Light high-strength multilayer nanofiber composite material and preparation method thereof Download PDFInfo
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- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
- D04H1/54—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties by welding together the fibres, e.g. by partially melting or dissolving
- D04H1/541—Composite fibres, e.g. sheath-core, sea-island or side-by-side; Mixed fibres
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- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
- B32B37/10—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the pressing technique, e.g. using action of vacuum or fluid pressure
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B5/00—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts
- B32B5/02—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by structural features of a fibrous or filamentary layer
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- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B5/00—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts
- B32B5/22—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed
- B32B5/24—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed one layer being a fibrous or filamentary layer
- B32B5/26—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed one layer being a fibrous or filamentary layer another layer next to it also being fibrous or filamentary
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- 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
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
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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
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
- D01F6/90—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of polyamides
- D01F6/905—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of polyamides of aromatic polyamides
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- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
- D04H1/54—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties by welding together the fibres, e.g. by partially melting or dissolving
- D04H1/559—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties by welding together the fibres, e.g. by partially melting or dissolving the fibres being within layered webs
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- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/70—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres
- D04H1/72—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged
- D04H1/728—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged by electro-spinning
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M17/00—Producing multi-layer textile fabrics
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2262/00—Composition or structural features of fibres which form a fibrous or filamentary layer or are present as additives
- B32B2262/02—Synthetic macromolecular fibres
- B32B2262/0223—Vinyl resin fibres
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2262/00—Composition or structural features of fibres which form a fibrous or filamentary layer or are present as additives
- B32B2262/02—Synthetic macromolecular fibres
- B32B2262/0253—Polyolefin fibres
Abstract
The invention provides a light high-strength multilayer nanofiber composite material which comprises an enhanced PMIA electrostatic spinning nanofiber layer and an enhanced PAN electrostatic spinning nanofiber layer which are alternately superposed, wherein CNF is adopted as a reinforcing agent in both the enhanced PMIA electrostatic spinning nanofiber layer and the enhanced PAN electrostatic spinning nanofiber layer. The multilayer nanofiber three-dimensional structure material comprising the enhanced PMIA electrospun nanofiber layer and the enhanced PAN electrospun nanofiber layer which are alternately stacked is prepared by combining the electrospinning technology with the hot pressing treatment process, integrates the excellent performances of PMIA, PAN and CNF, and is a three-dimensional structure function integrated nanofiber composite material with light weight, high strength and excellent impact resistance.
Description
Technical Field
The invention relates to the technical field of high polymer materials, in particular to a light high-strength multilayer nanofiber composite material and a preparation method thereof.
Background
The nano fiber has the characteristics of light weight, large specific surface area, high porosity and the like, and thus the method can expose the head and corners in the field of composite material application. In recent years, many researchers have tried to improve the nano-scale performance to the macroscopic level, but to date, the nano-fibers are made into macroscopic fibers or films, such as sensor sensing films, protective clothing materials, conductive and reinforcing materials, and these thin-film materials made of nano-fibers have defects in impact resistance and are difficult to meet the application requirements in many fields (such as structural members). With the development of science and technology, light-weight high-strength structural materials become an important research direction of modern advanced materials. At present, light, super-strong and impact-resistant structural materials are urgently needed in the fields of transportation, packaging, construction, automobiles, aerospace and the like. Particularly, after the 21 st century, under the promotion of the high-speed development of global industrialization, the fields of design, production, manufacturing and the like of light high-strength impact-resistant structural materials are well developed, and great changes are brought to human life, production activities and the like.
The aramid fiber 1313(PMIA) is an organic polymer fiber synthesized from isophthaloyl dichloride and m-phenylenediamine. The PMIA fiber has excellent heat resistance, flame retardance, chemical stability, electrical insulation, radiation resistance and good mechanical properties (light weight, good strength, strength 5-6 times that of steel, modulus twice that of steel and weight 1/5 of steel), so that the PMIA fiber can be used for manufacturing special functional materials, is suitable for severe environments such as high temperature, high humidity and the like, and has wide application in the fields of aerospace, national defense industry, transportation, electrical insulation and the like.
However, the strength of PMIA is not as high as that of aramid fiber 1414, so in order to prepare a three-dimensional functional structure composite material with high strength, a reinforcing agent must be added to meet the requirement of ultrahigh strength. Cellulose nanofibers (CNF for short) have many advantages, such as high strength, high elastic modulus, reproducibility, low density, and can be used as reinforcing materials and fillers to manufacture environment-friendly products.
Polyacrylonitrile (PAN for short) is prepared from acrylonitrile monomer (-CH)2The nitrile group on the surface of the high molecular polymer polymerized from-CH-C [ identical to ] N-' has stronger activity. Although the strength of PAN is not high, PAN has excellent weather resistance and sun exposure resistance, can still maintain about 77% of the original strength after being placed outdoors for 18 months, and is resistant to chemical agents, particularly inorganic acids, hydrogen peroxide, bleaching powder and general organic agents.
If the performance advantages of the materials can be combined, the excellent performances of the materials can be enhanced and fully exerted, and the problem of poor impact resistance of a film made of the nano fibers can be solved, so that the three-dimensional structure function integrated nano fiber composite material which takes PMIA, PAN and CNF as raw materials and has light weight, high strength and excellent impact resistance can be prepared, the development of the nano fibers can be promoted, the application field of the nano fibers can be enlarged, and the use requirements of structural members can be better met.
Disclosure of Invention
In view of the above, the invention provides a light high-strength multilayer nanofiber composite material and a preparation method thereof.
The invention provides a light high-strength multilayer nanofiber composite material which comprises an enhanced PMIA electrostatic spinning nanofiber layer and an enhanced PAN electrostatic spinning nanofiber layer which are alternately superposed; CNF is adopted as a reinforcing agent in both the enhanced PMIA electrospun nanofiber layer and the enhanced PAN electrospun nanofiber layer.
Further, the thickness of the nanofiber composite material is 0.5-10 mm.
Further, the electrospinning solution A for preparing the enhanced PMIA electrospinning nanofiber layer comprises the following raw material components in parts by weight: 10-16 parts of PMIA pulp, 3.3-9.9 parts of LiCl, 84-90 parts of organic solvent I and 0.1-1.6 parts of CNF;
the electrostatic spinning solution B for preparing the enhanced PAN electrostatic spinning nanofiber layer comprises the following raw material components in parts by weight: 10-16 parts of PAN fiber, 84-90 parts of organic solvent II and 0.1-1.6 parts of CNF.
Further, the organic solvent I and the organic solvent II are one or a mixture of N, N-dimethylacetamide, N-dimethylformamide and dimethyl sulfoxide.
The invention also provides a preparation method of the light high-strength multilayer nanofiber composite material, which comprises the following steps:
(1) preparing LiCl and an organic solvent I into a mixed solution, then adding PMIA pulp into the mixed solution, placing the mixed solution in a constant-temperature oil bath kettle and stirring until PMIA fibers are completely dissolved, then adding CNF into the obtained solution, placing the solution in the constant-temperature oil bath kettle and stirring until the CNF is uniformly dispersed, and obtaining an electrostatic spinning solution A;
uniformly mixing PAN fiber and an organic solvent II, placing the mixture in a constant-temperature oil bath kettle, stirring until the PAN fiber is completely dissolved, then adding CNF into the obtained solution, placing the solution in the constant-temperature oil bath kettle, and stirring until the CNF is uniformly dispersed to prepare an electrostatic spinning solution B;
(2) carrying out electrostatic spinning on the electrostatic spinning solution A and the electrostatic spinning solution B, respectively stacking the electrostatic spinning solution A and the electrostatic spinning solution B on a receiver device to form an enhanced PMIA electrostatic spinning nanofiber layer and an enhanced PAN electrostatic spinning nanofiber layer, and then slightly uncovering the enhanced PMIA electrostatic spinning nanofiber layer and the enhanced PAN electrostatic spinning nanofiber layer;
(3) and (3) alternately superposing the enhanced PMIA electrostatic spinning nanofiber layer and the enhanced PAN electrostatic spinning nanofiber layer obtained in the step (2), and then carrying out hot pressing treatment to obtain the light high-strength multilayer nanofiber composite material.
Further, in the step (1), the temperature of the constant-temperature oil bath is controlled to be 50-80 ℃.
Further, in the step (2), the specific conditions of electrostatic spinning are as follows: under the conditions of 20-28 ℃ and 20-70% of relative humidity, the flow rate of the electrostatic spinning solution is 0.3-5 mL/h, the distance between a spinning nozzle and a receiver device is 5-30 cm, and the spinning voltage is 10-30 kV.
Further, in the step (3), the temperature of the hot pressing treatment is controlled to be 50-200 ℃, the pressure is controlled to be 5-100 MPa, and the pressure maintaining time is 30-240 s.
The invention has the beneficial effects that:
according to the invention, the multilayer nanofiber three-dimensional structure material comprising the enhanced PMIA electrospun nanofiber layer and the enhanced PAN electrospun nanofiber layer which are alternately stacked is prepared by combining the electrostatic spinning process with the hot pressing process, integrates the excellent performances of PMIA, PAN and CNF, and is a three-dimensional structure function integrated nanofiber composite material with light weight, high strength and excellent impact resistance. Through the alternate superposition of the enhanced PMIA electrostatic spinning nanofiber layer and the enhanced PAN electrostatic spinning nanofiber layer, the phenomenon that the strength of the material is reduced due to stress concentration when the material receives external force is avoided, the energy can be absorbed when the material is impacted by external high energy, and meanwhile, the excellent strength is kept, so that the material is a potential shock wave armor material. Meanwhile, parts or structural components with different shapes and sizes can be obtained by machine tool processing, and the defect that the traditional nanofiber membrane is weak in impact resistance is overcome. The CNF is utilized to enhance the hydrogen bond connection between the PMIA nano fiber and the PAN nano fiber, so that the mechanical property of the multilayer nano fiber three-dimensional structure material is improved. In addition, compared with the mode that PMIA electrostatic spinning nanofiber layers are completely adopted for superposition, the enhanced PMIA electrostatic spinning nanofiber layers and the enhanced PAN electrostatic spinning nanofiber layers are alternately superposed, so that the function is more comprehensive, and the material cost is reduced.
The nano-fiber composite material provided by the invention has the tensile strength of 80-300 MPa and the density of 0.3-2.0 g/cm3The impact absorption energy is 0.5 to 12 kJ.m-1The high-strength high-impact-resistance support material is light in weight, has excellent strength and impact resistance, is expected to play a role in light-weight high-strength impact-resistance support materials required by automobiles, high-speed rails and aerospace, and provides more material choices for engineering design.
Drawings
The invention is further described below with reference to the following figures and examples:
FIG. 1 is a flow chart of the preparation of the light weight, high strength multi-layer nanofiber composite of the present invention.
Detailed Description
Example one
The embodiment provides a light-weight high-strength multilayer nanofiber composite material with the thickness of 0.5mm, which comprises enhanced PMIA electrospun nanofiber layers and enhanced PAN electrospun nanofiber layers which are alternately stacked.
In this example, the electrospinning solution a for preparing the enhanced PMIA electrospinning nanofiber layer comprises the following raw material components in parts by weight: 10 parts of PMIA pulp, 3.3 parts of LiCl, 90 parts of N, N-dimethylacetamide and 0.1 part of CNF;
the electrostatic spinning solution B for preparing the enhanced PAN electrostatic spinning nanofiber layer comprises the following raw material components in parts by weight: 10 parts of PAN fiber, 90 parts of N, N-dimethylacetamide and 0.1 part of CNF.
The preparation method of the light-weight high-strength multilayer nanofiber composite material provided by the embodiment comprises the following steps:
(1) preparing LiCl and N, N-dimethylacetamide into a mixed solution, adding dry PMIA pulp into the mixed solution, placing the mixed solution in a constant-temperature oil bath kettle at the temperature of 50 ℃ and stirring for 120 minutes until PMIA fibers are completely dissolved, then adding CNF into the obtained solution, placing the solution in a constant-temperature oil bath kettle at the temperature of 50 ℃ and stirring until the CNF is uniformly dispersed to prepare an electrostatic spinning solution A;
uniformly mixing PAN fiber and N, N-dimethylacetamide, placing the mixture in a constant-temperature oil bath kettle at the temperature of 50 ℃ and stirring for 60 minutes until the PAN fiber is completely dissolved, then adding CNF into the obtained solution, placing the solution in the constant-temperature oil bath kettle at the temperature of 50 ℃ and stirring until the CNF is uniformly dispersed to prepare an electrostatic spinning solution B;
(2) performing electrostatic spinning on the electrostatic spinning solution a and the electrostatic spinning solution B, respectively stacking and forming an enhanced PMIA electrostatic spinning nanofiber layer and an enhanced PAN electrostatic spinning nanofiber layer on a receiver device (the receiving device adopted in the embodiment is a flat-plate receiver, or a drum receiver), and then slightly removing the enhanced PMIA electrostatic spinning nanofiber layer and the enhanced PAN electrostatic spinning nanofiber layer; the specific conditions of electrostatic spinning are as follows: under the conditions of 23 ℃ and 25% of relative humidity, the flow rate of the electrostatic spinning solution is 0.6mL/h, the distance between a spinning nozzle and a receiver device is 12cm, and the spinning voltage is 15 kV;
(3) alternately superposing the enhanced PMIA electrostatic spinning nanofiber layer and the enhanced PAN electrostatic spinning nanofiber layer obtained in the step (2), and then carrying out hot pressing treatment to obtain a light high-strength multilayer nanofiber composite material; and during hot pressing, the temperature of a hot press adopted for hot pressing is controlled to be 50 ℃, the pressure is controlled to be 100MPa, and the pressure maintaining time is 240 s.
Example two
The embodiment provides a light-weight high-strength multilayer nanofiber composite material with the thickness of 2mm, which comprises enhanced PMIA electrospun nanofiber layers and enhanced PAN electrospun nanofiber layers which are alternately stacked.
In this example, the electrospinning solution a for preparing the enhanced PMIA electrospinning nanofiber layer comprises the following raw material components in parts by weight: PMIA pulp 12 parts, LiCl 6 parts, N-dimethylformamide 88 parts, CNF 0.15 parts;
the electrostatic spinning solution B for preparing the enhanced PAN electrostatic spinning nanofiber layer comprises the following raw material components in parts by weight: 12 parts of PAN fiber, 88 parts of N, N-dimethylformamide and 0.15 part of CNF.
The preparation method of the light-weight high-strength multilayer nanofiber composite material provided by the embodiment comprises the following steps:
(1) preparing LiCl and N, N-dimethylformamide into a mixed solution, adding dry PMIA pulp into the mixed solution, placing the mixed solution in a constant-temperature oil bath kettle at the temperature of 60 ℃ and stirring for 120 minutes until PMIA fibers are completely dissolved, then adding CNF into the obtained solution, placing the solution in a constant-temperature oil bath kettle at the temperature of 60 ℃ and stirring until CNF is uniformly dispersed to prepare an electrostatic spinning solution A;
uniformly mixing PAN fiber and N, N-dimethylformamide, placing the mixture in a constant-temperature oil bath kettle at the temperature of 60 ℃ and stirring for 60 minutes until the PAN fiber is completely dissolved, then adding CNF into the obtained solution, placing the solution in the constant-temperature oil bath kettle at the temperature of 60 ℃ and stirring until the CNF is uniformly dispersed to obtain an electrostatic spinning solution B;
(2) performing electrostatic spinning on the electrostatic spinning solution a and the electrostatic spinning solution B, respectively stacking and forming an enhanced PMIA electrostatic spinning nanofiber layer and an enhanced PAN electrostatic spinning nanofiber layer on a receiver device (the receiving device adopted in the embodiment is a flat-plate receiver, or a drum receiver), and then slightly removing the enhanced PMIA electrostatic spinning nanofiber layer and the enhanced PAN electrostatic spinning nanofiber layer; the specific conditions of electrostatic spinning are as follows: under the conditions of 23 ℃ and 25% of relative humidity, the flow rate of the electrostatic spinning solution is 0.5mL/h, the distance between a spinning nozzle and a receiver device is 15cm, and the spinning voltage is 15 kV;
(3) alternately superposing the enhanced PMIA electrostatic spinning nanofiber layer and the enhanced PAN electrostatic spinning nanofiber layer obtained in the step (2), and then carrying out hot pressing treatment to obtain a light high-strength multilayer nanofiber composite material; and during hot pressing, the temperature of a hot press adopted for hot pressing is controlled to be 90 ℃, the pressure is controlled to be 80MPa, and the pressure maintaining time is 200 s.
EXAMPLE III
The embodiment provides a light-weight high-strength multilayer nanofiber composite material with the thickness of 4mm, which comprises enhanced PMIA electrospun nanofiber layers and enhanced PAN electrospun nanofiber layers which are alternately stacked.
In this example, the electrospinning solution a for preparing the enhanced PMIA electrospinning nanofiber layer comprises the following raw material components in parts by weight: PMIA pulp 16 parts, LiCl 9.9 parts, N-dimethylacetamide 84 parts, CNF 0.32 parts;
the electrostatic spinning solution B for preparing the enhanced PAN electrostatic spinning nanofiber layer comprises the following raw material components in parts by weight: 16 parts of PAN fiber, 84 parts of dimethyl sulfoxide and 0.32 part of CNF.
The preparation method of the light-weight high-strength multilayer nanofiber composite material provided by the embodiment comprises the following steps:
(1) preparing LiCl and N, N-dimethylacetamide into a mixed solution, adding dry PMIA pulp into the mixed solution, placing the mixed solution in a constant-temperature oil bath kettle at the temperature of 80 ℃ and stirring for 120 minutes until PMIA fibers are completely dissolved, then adding CNF into the obtained solution, placing the solution in a constant-temperature oil bath kettle at the temperature of 80 ℃ and stirring until the CNF is uniformly dispersed to prepare an electrostatic spinning solution A;
uniformly mixing PAN fiber and dimethyl sulfoxide, placing the mixture in a constant-temperature oil bath kettle at the temperature of 80 ℃ and stirring for 60 minutes until the PAN fiber is completely dissolved, then adding CNF into the obtained solution, placing the solution in a constant-temperature oil bath kettle at the temperature of 80 ℃ and stirring until the CNF is uniformly dispersed to prepare an electrostatic spinning solution B;
(2) performing electrostatic spinning on the electrostatic spinning solution a and the electrostatic spinning solution B, respectively stacking and forming an enhanced PMIA electrostatic spinning nanofiber layer and an enhanced PAN electrostatic spinning nanofiber layer on a receiver device (the receiving device adopted in the embodiment is a flat-plate receiver, or a drum receiver), and then slightly removing the enhanced PMIA electrostatic spinning nanofiber layer and the enhanced PAN electrostatic spinning nanofiber layer; the specific conditions of electrostatic spinning are as follows: under the conditions of 23 ℃ and 25% of relative humidity, the flow rate of the electrostatic spinning solution is 0.6mL/h, the distance between a spinning nozzle and a receiver device is 15cm, and the spinning voltage is 20 kV;
(3) alternately superposing the enhanced PMIA electrostatic spinning nanofiber layer and the enhanced PAN electrostatic spinning nanofiber layer obtained in the step (2), and then carrying out hot pressing treatment to obtain a light high-strength multilayer nanofiber composite material; and during hot pressing, the temperature of a hot press adopted for hot pressing is controlled to be 130 ℃, the pressure is 50MPa, and the pressure maintaining time is 160 s.
Example four
The embodiment provides a light-weight high-strength impact-resistant nanofiber composite material with the thickness of 7mm, which comprises an enhanced PMIA electrospun nanofiber layer and an enhanced PAN electrospun nanofiber layer which are alternately stacked.
In this example, the electrospinning solution a for preparing the enhanced PMIA electrospinning nanofiber layer comprises the following raw material components in parts by weight: PMIA pulp 14 parts, LiCl 8 parts, N-dimethylacetamide 86 parts, CNF 0.467 parts;
the electrostatic spinning solution B for preparing the enhanced PAN electrostatic spinning nanofiber layer comprises the following raw material components in parts by weight: 14 parts of PAN fiber, 86 parts of N, N-dimethylacetamide and 0.467 part of CNF.
The preparation method of the light-weight high-strength multilayer nanofiber composite material provided by the embodiment comprises the following steps:
(1) preparing LiCl and N, N-dimethylacetamide into a mixed solution, adding dry PMIA pulp into the mixed solution, placing the mixed solution in a constant-temperature oil bath kettle at the temperature of 80 ℃ and stirring for 120 minutes until PMIA fibers are completely dissolved, then adding CNF into the obtained solution, placing the solution in a constant-temperature oil bath kettle at the temperature of 80 ℃ and stirring until the CNF is uniformly dispersed to prepare an electrostatic spinning solution A;
uniformly mixing PAN fiber and N, N-dimethylacetamide, placing the mixture in a constant-temperature oil bath kettle at the temperature of 60 ℃ and stirring for 60 minutes until the PAN fiber is completely dissolved, then adding CNF into the obtained solution, placing the solution in the constant-temperature oil bath kettle at the temperature of 60 ℃ and stirring until the CNF is uniformly dispersed to obtain an electrostatic spinning solution B;
(2) performing electrostatic spinning on the electrostatic spinning solution a and the electrostatic spinning solution B, respectively stacking and forming an enhanced PMIA electrostatic spinning nanofiber layer and an enhanced PAN electrostatic spinning nanofiber layer on a receiver device (the receiving device adopted in the embodiment is a flat-plate receiver, or a drum receiver), and then slightly removing the enhanced PMIA electrostatic spinning nanofiber layer and the enhanced PAN electrostatic spinning nanofiber layer; the specific conditions of electrostatic spinning are as follows: under the conditions of 23 ℃ and 25% of relative humidity, the flow rate of the electrostatic spinning solution is 0.6mL/h, the distance between a spinning nozzle and a receiver device is 15cm, and the spinning voltage is 20 kV;
(3) alternately superposing the enhanced PMIA electrostatic spinning nanofiber layer and the enhanced PAN electrostatic spinning nanofiber layer obtained in the step (2), and then carrying out hot pressing treatment to obtain a light high-strength multilayer nanofiber composite material; and during hot pressing, the temperature of a hot press adopted for hot pressing is controlled to be 200 ℃, the pressure is controlled to be 5MPa, and the pressure maintaining time is 100 s.
EXAMPLE five
The embodiment provides a light-weight high-strength impact-resistant nanofiber composite material with the thickness of 10mm, which comprises enhanced PMIA electrospun nanofiber layers and enhanced PAN electrospun nanofiber layers which are alternately stacked.
In this example, the electrospinning solution a for preparing the enhanced PMIA electrospinning nanofiber layer comprises the following raw material components in parts by weight: 10 parts of PMIA pulp, 4 parts of LiCl, 90 parts of N, N-dimethylacetamide and 1 part of CNF;
the electrostatic spinning solution B for preparing the enhanced PAN electrostatic spinning nanofiber layer comprises the following raw material components in parts by weight: 10 parts of PAN fiber, 90 parts of N, N-dimethylacetamide and 1 part of CNF.
The preparation method of the light-weight high-strength multilayer nanofiber composite material provided by the embodiment comprises the following steps:
(1) preparing LiCl and N, N-dimethylacetamide into a mixed solution, adding dry PMIA pulp into the mixed solution, placing the mixed solution in a constant-temperature oil bath kettle at the temperature of 80 ℃ and stirring for 120 minutes until PMIA fibers are completely dissolved, then adding CNF into the obtained solution, placing the solution in a constant-temperature oil bath kettle at the temperature of 80 ℃ and stirring until the CNF is uniformly dispersed to prepare an electrostatic spinning solution A;
uniformly mixing PAN fiber and N, N-dimethylacetamide, placing the mixture in a constant-temperature oil bath kettle at the temperature of 60 ℃ and stirring for 60 minutes until the PAN fiber is completely dissolved, then adding CNF into the obtained solution, placing the solution in the constant-temperature oil bath kettle at the temperature of 60 ℃ and stirring until the CNF is uniformly dispersed to obtain an electrostatic spinning solution B;
(2) performing electrostatic spinning on the electrostatic spinning solution a and the electrostatic spinning solution B, respectively stacking and forming an enhanced PMIA electrostatic spinning nanofiber layer and an enhanced PAN electrostatic spinning nanofiber layer on a receiver device (the receiving device adopted in the embodiment is a flat-plate receiver, or a drum receiver), and then slightly removing the enhanced PMIA electrostatic spinning nanofiber layer and the enhanced PAN electrostatic spinning nanofiber layer; the specific conditions of electrostatic spinning are as follows: under the conditions of 23 ℃ and 25% of relative humidity, the flow rate of the electrostatic spinning solution is 0.6mL/h, the distance between a spinning nozzle and a receiver device is 15cm, and the spinning voltage is 15 kV;
(3) alternately superposing the enhanced PMIA electrostatic spinning nanofiber layer and the enhanced PAN electrostatic spinning nanofiber layer obtained in the step (2), and then carrying out hot pressing treatment to obtain a light high-strength multilayer nanofiber composite material; and during hot pressing, the temperature of a hot press adopted for hot pressing is controlled to be 170 ℃, the pressure is controlled to be 20MPa, and the pressure maintaining time is 30 s.
The properties of the multilayer nanofiber composites prepared in examples one-five were tested and the results are shown in the following table:
from the above table, the nanofiber composite material prepared by the invention is a three-dimensional structure composite material with light weight, high strength and excellent impact resistance.
Finally, the above embodiments are only for illustrating the technical solutions of the present invention and not for limiting, although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions may be made to the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention, and all of them should be covered in the claims of the present invention.
Claims (8)
1. A light high-strength multilayer nanofiber composite material is characterized in that: comprises an enhanced PMIA electrostatic spinning nanofiber layer and an enhanced PAN electrostatic spinning nanofiber layer which are alternately superposed.
2. The light weight, high strength multilayer nanofiber composite of claim 1, characterized in that: the thickness of the nanofiber composite material is 0.5-10 mm.
3. The light weight, high strength multilayer nanofiber composite of claim 1, characterized in that: the electrostatic spinning solution A for preparing the enhanced PMIA electrostatic spinning nanofiber layer comprises the following raw material components in parts by weight: 10-16 parts of PMIA pulp, 3.3-9.9 parts of LiCl, 84-90 parts of organic solvent I and 0.1-1.6 parts of CNF;
the electrostatic spinning solution B for preparing the enhanced PAN electrostatic spinning nanofiber layer comprises the following raw material components in parts by weight: 10-16 parts of PAN fiber, 84-90 parts of organic solvent II and 0.1-1.6 parts of CNF.
4. The light weight, high strength multilayer nanofiber composite of claim 3, characterized in that: the organic solvent I and the organic solvent II are one or a mixture of N, N-dimethylacetamide, N-dimethylformamide and dimethyl sulfoxide.
5. A preparation method of a light high-strength multilayer nanofiber composite material is characterized by comprising the following steps: the method comprises the following steps:
(1) preparing LiCl and an organic solvent I into a mixed solution, then adding PMIA pulp into the mixed solution, placing the mixed solution in a constant-temperature oil bath kettle and stirring until PMIA fibers are completely dissolved, then adding CNF into the obtained solution, placing the solution in the constant-temperature oil bath kettle and stirring until the CNF is uniformly dispersed, and obtaining an electrostatic spinning solution A;
uniformly mixing PAN fiber and an organic solvent II, placing the mixture in a constant-temperature oil bath kettle, stirring until the PAN fiber is completely dissolved, then adding CNF into the obtained solution, placing the solution in the constant-temperature oil bath kettle, and stirring until the CNF is uniformly dispersed to prepare an electrostatic spinning solution B;
(2) carrying out electrostatic spinning on the electrostatic spinning solution A and the electrostatic spinning solution B, respectively stacking the electrostatic spinning solution A and the electrostatic spinning solution B on a receiver device to form an enhanced PMIA electrostatic spinning nanofiber layer and an enhanced PAN electrostatic spinning nanofiber layer, and then slightly uncovering the enhanced PMIA electrostatic spinning nanofiber layer and the enhanced PAN electrostatic spinning nanofiber layer;
(3) and (3) alternately superposing the enhanced PMIA electrostatic spinning nanofiber layer and the enhanced PAN electrostatic spinning nanofiber layer obtained in the step (2), and then carrying out hot pressing treatment to obtain the light high-strength multilayer nanofiber composite material.
6. The preparation method of the light-weight high-strength multilayer nanofiber composite material as claimed in claim 5, wherein the preparation method comprises the following steps: in the step (1), the temperature of the constant-temperature oil bath is controlled to be 50-80 ℃.
7. The preparation method of the light-weight high-strength multilayer nanofiber composite material as claimed in claim 5, wherein the preparation method comprises the following steps: in the step (2), the specific conditions of electrostatic spinning are as follows: under the conditions of 20-28 ℃ and 20-70% of relative humidity, the flow rate of the electrostatic spinning solution is 0.3-5 mL/h, the distance between a spinning nozzle and a receiver device is 5-30 cm, and the spinning voltage is 10-30 kV.
8. The preparation method of the light-weight high-strength multilayer nanofiber composite material as claimed in claim 5, wherein the preparation method comprises the following steps: in the step (3), the temperature of the hot pressing treatment is controlled to be 50-200 ℃, the pressure is controlled to be 5-100 MPa, and the pressure maintaining time is 30-240 s.
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