CN111172672B - MXenes/polyurethane thermal insulation material and preparation method thereof - Google Patents
MXenes/polyurethane thermal insulation material and preparation method thereof Download PDFInfo
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- CN111172672B CN111172672B CN202010049597.4A CN202010049597A CN111172672B CN 111172672 B CN111172672 B CN 111172672B CN 202010049597 A CN202010049597 A CN 202010049597A CN 111172672 B CN111172672 B CN 111172672B
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- MTPVUVINMAGMJL-UHFFFAOYSA-N trimethyl(1,1,2,2,2-pentafluoroethyl)silane Chemical compound C[Si](C)(C)C(F)(F)C(F)(F)F MTPVUVINMAGMJL-UHFFFAOYSA-N 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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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
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D10/00—Physical treatment of artificial filaments or the like during manufacture, i.e. during a continuous production process before the filaments have been collected
- D01D10/06—Washing or drying
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/0007—Electro-spinning
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/0007—Electro-spinning
- D01D5/0015—Electro-spinning characterised by the initial state of the material
- D01D5/003—Electro-spinning characterised by the initial state of the material the material being a polymer solution or dispersion
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/0007—Electro-spinning
- D01D5/0061—Electro-spinning characterised by the electro-spinning apparatus
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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
- 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
- D01F1/07—Addition of substances to the spinning solution or to the melt for making fire- or flame-proof filaments
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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
- 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
- D01F1/09—Addition of substances to the spinning solution or to the melt for making electroconductive or anti-static filaments
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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
- D01F6/44—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds
- D01F6/48—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds of polymers of halogenated hydrocarbons
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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
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
- D01F8/12—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyamide as constituent
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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
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
- D01F8/16—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one other macromolecular compound obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds as constituent
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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
- D04H3/00—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length
- D04H3/02—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length characterised by the method of forming fleeces or layers, e.g. reorientation of yarns or filaments
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- D10—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B2401/00—Physical properties
- D10B2401/16—Physical properties antistatic; conductive
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
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- Dispersion Chemistry (AREA)
- Artificial Filaments (AREA)
Abstract
The invention relates to preparation of a composite material, and particularly relates to an MXenes/polyurethane thermal insulation material and a preparation method thereof. The preparation method of the material comprises the following steps: the preparation method comprises the steps of adopting an electrostatic melt-blowing technology, blowing and spinning polyurethane mixed liquor containing different contents of polysulfonamide fibers and flame retardants into fibrous foam by utilizing high voltage and air pressure, and then combining MXenes with the prepared flame-retardant heat-insulating material through electrostatic spinning to prepare the novel heat-insulating material with flame retardance and electromagnetic shielding performance. The material has the beneficial properties of good heat preservation, excellent flame retardance, good electromagnetic shielding and the like, and overcomes the defects of flammability, lack of electromagnetic shielding and toxic gas generation in combustion of the traditional heat preservation material. Can be adjusted according to different use environments, has simple process, safe operation and excellent performance, and is suitable for large-scale production.
Description
Technical Field
The invention relates to preparation of a composite material, and particularly relates to an MXenes/polyurethane thermal insulation material and a preparation method thereof.
Background
The polyurethane foam material has excellent heat preservation and sound absorption performance, so that the polyurethane foam material is widely applied to the fields of heat preservation of automobiles, furniture, building walls and the like. Rigid polyurethane foams readily decompose in air and produce large quantities of combustible microscopic debris. The fragments spread to the surface of polyurethane and mix with air, and have strong flammability. Meanwhile, rigid polyurethane foams release a large amount of toxic gases such as: low molecular weight hydrocarbons, CO2HCN, etc. These toxic fumes can be inhaled by the human body and pose a potential health hazard, which is also a major cause of death in a fire. Therefore, rigid polyurethane foams are improvedThe flame retardancy of (2) is imperative. Flame retardancy refers to the property of a substance or material that, after treatment, has a significant delay in the spread of a flame.
Currently, combustible materials are usually given certain flame retardant properties by adding flame retardants, and most of the used flame retardants include halogen-based flame retardants and inorganic flame retardants. Halogen-based flame retardants are inexpensive and have a good flame retardant effect, and thus they have a wide market, but they generate a large amount of gas harmful to the body when burned. The inorganic flame retardant has the characteristics of low price and low toxicity, but the flame retardant property is poor, and the LOI can reach 26 percent only by adding excessive inorganic compounds. In addition, excessive flame retardant can affect the mechanical properties of materials and the polymer forming process, and has a large influence on the mechanical properties of the base material. The phosphorus flame retardant can act in a gas phase and can also act in a condensed phase, and toxic gas is not generated in the combustion process. Therefore, phosphorus-based flame retardants have been drawing attention.
In recent years, electronic devices have been developed to be smaller, lighter, and more reliable due to the development of scientific technology and the direction of human demand, which requires higher power and faster operation of portable electronic devices. However, electronic devices radiate large amounts of high frequency electromagnetic waves, such as microwaves and radio frequency electromagnetic waves, when operated at high power and high speed. The electromagnetic interference can influence the normal work of electronic devices, reduce the service life of equipment, and can directly interrupt the operation of the equipment when serious, thereby causing the damage of instruments. For the automobile field, electromagnetic interference can affect a GPS system, even a control system can be out of order, and serious traffic accidents are caused; for medical and laboratory instruments, electromagnetic interference can affect the normal operation of the equipment. The major effects of electromagnetic radiation on living bodies are due to dysfunction of the central nervous system and autonomic nervous disorders dominated by sympathetic fatigue and tone. Therefore, the solution to the problems of electromagnetic radiation and electromagnetic interference is not very slow.
The polysulfonamide fiber is a novel high-technology fiber product independently developed in China, and has excellent heat resistance, flame retardance and filtering performance, excellent physical and mechanical properties and excellent chemical stability. The long-term service temperature of the polysulfonamide fibers is 250 ℃, the strength retention rate is more than 80 percent after 100h heating, and the Limiting Oxygen Index (LOI) is 33 percent. Polysulfonamide is widely applied to the fields of protective products, building materials, aerospace, national defense war industry and the like, and is mixed with other fibers for use to make up for the defects of other fibers. The carbon fiber is a special fiber composed of carbon elements and has the characteristics of high temperature resistance, friction resistance, electric conduction, heat conduction, corrosion resistance and the like.
Recently, early transition metal carbides or carbonitrides (MXenes) have attracted attention as novel two-dimensional materials. MXenes were produced by etching away the A layer in the MAX phase. Mn+1AXnWherein M is an early transition metal, a is predominantly a group IIIA or IVA (i.e. group 13 or 14) element, X is C or N, and N is 1, 2 or 3. MXenes has good conductivity and large specific surface area, so that the MXenes can be used for energy storage, electromagnetic shielding and the like.
The polysulfonamide fiber has good flame retardant property and meets the requirement of the flame retardant material. From the flame-retardant nonwoven fabric, it can be processed into a flame-retardant nonwoven fabric by spinning, weaving, sizing, and the like. But the process is complicated.
The flame-retardant polyurethane heat-insulating material is prepared by adopting short polysulfonamide fibers, a phosphorus flame retardant, polyether polyol, isocyanate and a small amount of water at a certain content under a proper reaction temperature and time. Then MXenes and rigid polyurethane foam are compounded together through electrostatic spinning, and the thermal insulation material with excellent flame retardance and electromagnetic shielding performance is prepared through designing the structure of the polyurethane thermal insulation material, so that the thermal insulation material has important economic and social benefits.
Disclosure of Invention
The invention aims to solve the following primary technical problems: the ultrashort polysulfonamide fiber is uniformly embedded in the foam by controlling the ultrashort polysulfonamide fiber with different contents and changing the structure of the polyurethane foam heat-insulating material, so that the heat-insulating material with flame-retardant electromagnetic shielding performance, which is simple in process, safe to operate and excellent in performance, is prepared.
In order to achieve the purpose, the invention adopts the following technical scheme:
the MXenes/polyurethane thermal insulation material has the limiting oxygen index of 29-32% and the electromagnetic shielding value of 40-54 dB. MXenes has good metal conductivity as a new two-dimensional material (such as titanium carbide and the like); the polysulfonamide fiber contains sulfone group (═ SO) on the main chain of the molecular structure2) The material begins to decompose at the high temperature of above 420 ℃, so the material has better flame retardance and thermal stability; the thermal degradation product of the phosphorus flame retardant promotes the polymer surface to be rapidly dehydrated and carbonized, thereby forming a carbonized layer. The simple substance carbon does not carry out evaporation combustion and decomposition combustion for generating flame, so the flame-retardant carbon has a flame-retardant protection effect.
A preparation method of MXenes/polyurethane thermal insulation material comprises the following steps:
step 1, preparing a flame-retardant heat-insulating material spinning solution: taking polyether polyol and a phosphate flame retardant, stirring, uniformly mixing, standing to completely eliminate bubbles, slowly adding ultrashort aromatic polysulphone fibers, stirring, ultrasonically treating until the ultrashort aromatic polysulphone fibers are uniformly dispersed, standing to completely eliminate bubbles, slowly adding isocyanate, standing to slowly and uniformly mix the isocyanate to obtain a flame-retardant heat-insulation material spinning solution;
step 2, electrostatic melt-blown flame-retardant heat-insulating material: pouring the flame-retardant heat-insulating material spinning solution obtained in the step 1 into a melt-blowing die head of electrostatic melt-blowing equipment, paving a nylon fiber receiving net under the melt-blowing die head, under the action of high-voltage direct current and high-pressure air, spraying the flame-retardant heat-insulating material spinning solution obtained in the step 1 into a fiber bundle from a spinneret orifice, continuously observing whether the spinneret orifice is blocked or not in the melt-blowing process, dredging as soon as possible if the spinneret orifice is blocked, forming a layer of uniform and fluffy polyurethane fiber film on the surface of the nylon fiber receiving net after melt-blowing is finished, and then drying the polyurethane fiber film;
step 3, preparing electromagnetic shielding electrostatic spinning solution: mixing polyvinylidene fluoride and DMF/acetone, stirring, and slowly adding Ti3C2MXenes, stirred, then sonicated to Ti3C2MXenes is dispersed uniformly and kept stand to obtain electromagnetic shielding electrostatic spinning solution;
step 4, electrostatic spinning electromagnetic shielding flame-retardant heat-insulating material: injecting the electromagnetic shielding electrostatic spinning solution obtained in the step 3 into electrostatic spinning needle tube equipment, paving the polyurethane fiber membrane obtained in the step 2 on an electrostatic spinning aluminum foil receiver, spraying a fiber bundle from an electrostatic spinning head by the electromagnetic shielding electrostatic spinning solution obtained in the step 3 under the action of direct-current voltage, forming a black polyurethane fiber membrane on the electrostatic spinning aluminum foil receiver after electrostatic spinning is finished, and drying the black polyurethane fiber membrane to obtain the MXenes/polyurethane heat-insulating material. Generally, the shielding effectiveness is higher when the warp direction and the weft direction both contain metal fiber films, because the warp direction and the weft direction both contain metal fibers, which is equivalent to a complete criss-cross metal shielding conductive net formed in the fabric, so that the electromagnetic wave can be better prevented from being transmitted and the electromagnetic wave energy can be lost.
Further, in the step 1, the mass ratio of the polyether polyol to the phosphate ester flame retardant to the isocyanate is 15:3: 5-15, and the ultrashort polysulfonamide fiber is an ultrashort polysulfonamide fiber with the mass fraction of 0-7.5 wt%. Because air is a good insulating material, polyurethane foam has a high porosity: (>90%) so that a large amount of air can be stored with a small thermal conductivity and thus used for insulation. The polysulfonamide fiber contains sulfone group (═ SO) on the main chain of the molecular structure2) And the material begins to decompose at a high temperature of above 420 ℃, so that the material has better flame retardance and thermal stability.
Further, the stirring speed of the polyether polyol and the phosphate ester flame retardant in the step 1 is 1000-1200 rpm/min, and the stirring time is 10-15 min; adding the ultrashort polysulfonamide fibers, stirring at the rotating speed of 800-1200 rpm/min for 30-60 min. The mechanical stirring endows the solution with certain shearing force, and the extremely high stirring speed enables the shearing force to be larger than the surface tension of the polyether polyol and the phosphate ester, so that the polyether polyol and the phosphate ester flame retardant form uniform solution. The polysulfonamide fibers are also uniformly dispersed in the liquid by mechanical shear forces.
Further, in the step 2, the high-voltage direct current voltage is 38-40 KV, the wind pressure of high-pressure wind is 0.05-0.12 MPa, the temperature of the high-pressure wind is 23-26 ℃, the humidity of the high-pressure wind is 30-40%, the distance between the tip of a spinning nozzle of the melt-blowing die head and the nylon fiber receiving net is 800-1000 mm, the diameter of the spinning nozzle is 0.4mm, the melt-blowing time is 40-100 minutes, the drying temperature is 60-70 ℃, and the drying time is 4-6 hours. The electrostatic solution blowing technology is a novel nano-fiber preparation technology developed on the basis of the traditional electrostatic spinning, and the spinning solution is drawn and refined under the dual actions of an airflow field and an electrostatic field, so that the extrusion rate of the spinning solution is greatly accelerated, and the spinning efficiency and the yield of nano-microfibers are greatly improved. And the spun nanofiber web is in a three-dimensional network shape, the structure is fluffy, and the fibers can keep better flexibility in the high-temperature use process.
Further, in the step 3, polyvinylidene fluoride, DMF/acetone mixed solution and Ti are used3C2MXenes mass ratio 5.6:14.4:1, DMF to acetone volume ratio 7: 3. Polyvinylidene fluoride is easy to dissolve in DMF, and due to the fact that acetone is volatile in the electrostatic spinning process, the concentration of PVDF can be increased by a proper amount of acetone in the electrostatic spinning process, and therefore the viscosity of the solution is improved; due to good conductivity, Ti3C2MXenes can increase the conductivity of the solution, thereby facilitating electrostatic spinning.
Further, stirring the polyvinylidene fluoride and DMF/acetone mixed solution in the step 3 at the temperature of 45-55 ℃ and at the rotating speed of 20-25 rpm/min; adding Ti3C2The MXenes stirring time is 0.5-1 h, the stirring speed is 20-25 rpm/min, the stirring time is 30-40 min, and the standing time is 30-60 min. Due to the excellent bonding property, chemical resistance and high mechanical property of PVDF, MXenes can be grafted on the surface of the nanofiber, and the nanofiber can be well connected together to form a dense network structure so as to prevent electromagnetic waves from passing through.
Furthermore, in the step 4, the distance between the tip of the electrostatic spinning head of the electrostatic spinning needle tube equipment and the electrostatic spinning aluminum foil receiver is 160-200 mm, the direct current voltage is 25-32 KV, the temperature is 23-26 ℃, the humidity is 30-40%, the drying temperature is 60-70 ℃, and the drying time is 2-4 hours. Electrostatic spinning is a spinning process for drawing a polymer into nano fibers under the action of a strong electric field force, and is the only method for continuously producing the nano fibers at present. The solution is in the storage device, and can form liquid drops under the action of an electric field when an external electrode is arranged; or under the action of gravity, a liquid drop suspended at the pipe orifice is formed, charges are fully distributed on the surface of the liquid drop under the action of an electric field force, coulomb repulsion force borne by the liquid drop is opposite to the direction of surface tension of the liquid drop, when the electric field intensity is increased, the charge density on the surface of the liquid drop is increased, the coulomb repulsion force is larger than the surface tension of the liquid drop, the curvature of the liquid drop is changed, the liquid drop is stretched to form a cone, and the cone angle is 49.3 degrees, namely the charged liquid is. The Taylor cone is sprayed along with the increase of the voltage, the spraying flow is split under the action of the electric field, the spraying flow begins to solidify along with the slow volatilization of the solvent, and finally the formed nano fibers are collected on a receiving device.
Compared with the prior art, the invention has the following advantages: compounding a flame retardant, polysulfonamide fibers and a polyurethane solution into a novel flame-retardant heat-insulating material by utilizing electrostatic melt blowing, and compounding MXenes and the novel flame-retardant heat-insulating material by an electrostatic spinning method to prepare the heat-insulating material with flame retardance and electromagnetic shielding performance. The material has good flame retardant property, excellent electromagnetic shielding property and good heat insulation property, and overcomes the defects of flammability and lack of electromagnetic shielding property of the traditional heat insulation material.
Drawings
FIG. 1 is a representation of flame retardance and electromagnetic shielding of the novel flame-retardant and electromagnetic shielding heat-insulating material.
Detailed Description
Example 1
The preparation method of the MXenes/polyurethane thermal insulation material of the embodiment comprises the following steps:
step 1, preparing a flame-retardant heat-insulating material spinning solution: taking 15g of polyether polyol and 3g of phosphate flame retardant, stirring for 15min at 1000rpm/min by using an S569T2/A3 direct-current servo electric stirrer, uniformly mixing, standing to completely eliminate bubbles, slowly adding 2.5 mass percent of ultrashort aromatic polysulphone fibers at 800rpm/min, stirring for 60min, ultrasonically treating until the ultrashort aromatic polysulphone fibers are uniformly dispersed, standing to completely eliminate bubbles, slowly adding 5g of isocyanate, and standing to slowly and uniformly mix the isocyanate to obtain a flame-retardant and heat-insulating material spinning solution;
step 2, electrostatic melt-blown flame-retardant heat-insulating material: pouring the flame-retardant heat-insulating material spinning solution obtained in the step 1 into a melt-blowing die head of electrostatic melt-blowing equipment, paving a nylon fiber receiving net under the melt-blowing die head, wherein the distance between the tip of a spinneret of the melt-blowing die head and the nylon fiber receiving net is 800mm, under the action of high-voltage direct current and high-pressure air, a fiber bundle is sprayed out of the flame-retardant heat-insulating material spinning solution obtained in the step 1 from a spinneret hole with the diameter of 0.4mm, the voltage of the high-voltage direct current is 38KV, the pressure of the high-pressure air is 0.05MPa, the temperature of the high-pressure air is 23 ℃, the humidity of the high-pressure air is 30%, the melt-blowing time is 40min, after the melt-blowing is finished, a layer of uniform and fluffy polyurethane fiber film is formed on the surface of the nylon fiber receiving net, and then the polyurethane fiber film is placed into;
step 3, preparing electromagnetic shielding electrostatic spinning solution: taking 5.6g polyvinylidene fluoride and 14.4g DMF/acetone (volume ratio is 7:3) mixed solution, stirring for 1h at 45 ℃ under the magnetic force of 20rpm/min, and then slowly adding 1g Ti3C2MXenes, stirred at 20rpm/min for 40min, then sonicated to Ti3C2Uniformly dispersing MXenes, and standing for 30min to obtain electromagnetic shielding electrostatic spinning solution;
step 4, electrostatic spinning electromagnetic shielding flame-retardant heat-insulating material: injecting the electromagnetic shielding electrostatic spinning solution obtained in the step 3 into electrostatic spinning needle tube equipment, paving the polyurethane fiber membrane obtained in the step 2 on an electrostatic spinning aluminum foil receiver, enabling the distance between the tip of an electrostatic spinning head of the electrostatic spinning needle tube equipment and the electrostatic spinning aluminum foil receiver to be 160mm, spraying the electromagnetic shielding electrostatic spinning solution obtained in the step 3 out of a bundle of fiber bundles from the electrostatic spinning head under the action of direct current voltage, enabling the direct current voltage to be 25KV, the temperature to be 23 ℃ and the humidity to be 30%, forming a black polyurethane fiber membrane on the electrostatic spinning aluminum foil receiver after electrostatic spinning is completed, and then placing the black polyurethane fiber membrane into a blast oven to be dried for 4 hours at the temperature of 60 ℃ to obtain the MXenes/polyurethane heat-insulating material.
The MXenes/polyurethane thermal insulation material of the embodiment has the limiting oxygen index of 29-32% and the electromagnetic shielding value of 40-54 dB.
Example 2
The preparation method of the MXenes/polyurethane thermal insulation material with flame retardant and electromagnetic shielding performance comprises the following steps:
step 1, preparing a flame-retardant heat-insulating material spinning solution: taking 15g of polyether polyol and 3g of phosphate flame retardant, stirring for 13min at 1100rpm/min by using an S569T2/A3 direct-current servo electric stirrer, uniformly mixing, standing to completely eliminate bubbles, slowly adding 5 mass percent of ultrashort polysulfonamide fibers at 1000rpm/min, stirring for 45min, ultrasonically treating until the ultrashort polysulfonamide fibers are uniformly dispersed, standing to completely eliminate bubbles, slowly adding 10g of isocyanate, and standing to slowly and uniformly mix the isocyanate to obtain a flame-retardant heat-preservation material spinning solution;
step 2, electrostatic melt-blown flame-retardant heat-insulating material: pouring the flame-retardant heat-insulating material spinning solution obtained in the step 1 into a melt-blowing die head of electrostatic melt-blowing equipment, paving a nylon fiber receiving net under the melt-blowing die head, wherein the distance between the tip of a spinneret of the melt-blowing die head and the nylon fiber receiving net is 900mm, under the action of high-voltage direct current and high-pressure air, a fiber bundle is sprayed out of the flame-retardant heat-insulating material spinning solution obtained in the step 1 from a spinneret hole with the diameter of 0.4mm, the voltage of the high-voltage direct current is 39KV, the pressure of the high-pressure air is 0.08MPa, the temperature of the high-pressure air is 24 ℃, the humidity of the high-pressure air is 35%, the melt-blowing time is 70 minutes, after the melt-blowing is finished, a layer of uniform and fluffy polyurethane fiber film is formed on the surface of the nylon fiber receiving net, and then the polyurethane fiber film is placed into;
step 3, preparing electromagnetic shielding electrostatic spinning solution: taking a mixture of 5.6g polyvinylidene fluoride and 14.4g DMF/acetone (volume ratio of 7:3), magnetically stirring at 50 deg.C for 0.8h at 24rpm/min, and slowly adding 1g Ti3C2MXenes, stirred at 24rpm/min for 35min, then sonicated to Ti3C2Uniformly dispersing MXenes, and standing for 45min to obtain electromagnetic shielding electrostatic spinning solution;
step 4, electrostatic spinning electromagnetic shielding flame-retardant heat-insulating material: injecting the electromagnetic shielding electrostatic spinning solution obtained in the step 3 into electrostatic spinning needle tube equipment, paving the polyurethane fiber membrane obtained in the step 2 on an electrostatic spinning aluminum foil receiver, enabling the distance between the tip of an electrostatic spinning head of the electrostatic spinning needle tube equipment and the electrostatic spinning aluminum foil receiver to be 180mm, spraying the electromagnetic shielding electrostatic spinning solution obtained in the step 3 out of a bundle of fiber bundles from the electrostatic spinning head under the action of direct current voltage, enabling the direct current voltage to be 30KV, the temperature to be 25 ℃ and the humidity to be 35%, forming a black polyurethane fiber membrane on the electrostatic spinning aluminum foil receiver after electrostatic spinning is completed, and then placing the black polyurethane fiber membrane into a blast oven to be dried for 3 hours at 65 ℃ to obtain the MXenes/polyurethane heat-insulating material.
The MXenes/polyurethane thermal insulation material of the embodiment has the limiting oxygen index of 29-32% and the electromagnetic shielding value of 40-54 dB.
Example 3
The preparation method of the MXenes/polyurethane thermal insulation material of the embodiment comprises the following steps:
step 1, preparing a flame-retardant heat-insulating material spinning solution: taking 15g of polyether polyol and 3g of phosphate flame retardant, stirring for 10min at 1200rpm/min by using an S569T2/A3 direct-current servo electric stirrer, uniformly mixing, standing to completely eliminate bubbles, slowly adding 7.5 mass percent of ultrashort aromatic polysulphone fibers at 1200rpm/min, stirring for 30min, ultrasonically treating until the ultrashort aromatic polysulphone fibers are uniformly dispersed, standing to completely eliminate bubbles, slowly adding 15g of isocyanate, and standing to slowly and uniformly mix the isocyanate to obtain a flame-retardant and heat-insulating material spinning solution;
step 2, electrostatic melt-blown flame-retardant heat-insulating material: pouring the flame-retardant heat-insulating material spinning solution obtained in the step 1 into a melt-blowing die head of electrostatic melt-blowing equipment, paving a nylon fiber receiving net under the melt-blowing die head, wherein the distance between the tip of a spinneret of the melt-blowing die head and the nylon fiber receiving net is 1000mm, under the action of high-voltage direct current and high-pressure air, a fiber bundle is sprayed out of the flame-retardant heat-insulating material spinning solution obtained in the step 1 from a spinneret hole with the diameter of 0.4mm, the voltage of the high-voltage direct current is 40KV, the pressure of the high-pressure air is 0.12MPa, the temperature of the high-pressure air is 26 ℃, the humidity of the high-pressure air is 40%, the melt-blowing time is 70 minutes, after the melt-blowing is finished, a layer of uniform and fluffy polyurethane fiber film is formed on the surface of the nylon fiber receiving net, and then the polyurethane fiber film is placed into;
step 3, preparing electromagnetic shielding electrostatic spinning solution: taking 5.6g polyvinylidene fluoride and 14.4g DMF/acetone (volume ratio is 7:3) mixed solution, stirring for 0.5h at 55 ℃ under the magnetic force of 25rpm/min, and then slowly adding 1g Ti3C2MXenes, stirring at 25rpm/min for 30min, then sonicating to Ti3C2MXenes is dispersed uniformly and stands for 60min to obtain electromagnetic shielding electrostatic spinning solution;
step 4, electrostatic spinning electromagnetic shielding flame-retardant heat-insulating material: injecting the electromagnetic shielding electrostatic spinning solution obtained in the step 3 into electrostatic spinning needle tube equipment, paving the polyurethane fiber membrane obtained in the step 2 on an electrostatic spinning aluminum foil receiver, enabling the distance between the tip of an electrostatic spinning head of the electrostatic spinning needle tube equipment and the electrostatic spinning aluminum foil receiver to be 200mm, spraying the electromagnetic shielding electrostatic spinning solution obtained in the step 3 out of a bundle of fiber bundles from the electrostatic spinning head under the action of direct current voltage, enabling the direct current voltage to be 32KV, the temperature to be 26 ℃ and the humidity to be 40%, forming a black polyurethane fiber membrane on the electrostatic spinning aluminum foil receiver after electrostatic spinning is completed, and then placing the black polyurethane fiber membrane into a blast oven to be dried for 2 hours at 70 ℃ to obtain the MXenes/polyurethane heat-insulating material.
The MXenes/polyurethane thermal insulation material of the embodiment has the limiting oxygen index of 29-32% and the electromagnetic shielding value of 40-54 dB.
FIG. 1 shows Limiting Oxygen Index (LOI) and electromagnetic shielding patterns of polyurethane foams and novel insulation materials. As can be seen from the figure, the LOI value of the polyurethane foam is at least 17%, and it burns easily when exposed to fire. The novel thermal insulation material can improve the LOI value to 32 percent, and shows that: the novel heat-insulating material has good flame-retardant property. In the initial stage of combustion, P-O-C of the phosphorus-based flame retardant is broken and the char, which is a product of rapid decomposition, forms a dense carbon layer as heat and O2Thereby blocking heat transfer to the interior of the material. In addition, the polyurethane foam has less than 10dB of electromagnetic shielding and almost no electromagnetic shielding effect. The novel heat-insulating material has good conductivity by MXenes, and electromagnetic waves are reflected and absorbed after contacting the surface of the novel heat-insulating materialAnd multiple reflection, thereby achieving the purpose of attenuating the electromagnetic wave energy, further achieving more than 40dB, and having the effect of shielding the electromagnetic wave.
Claims (7)
1. The preparation method of the MXenes/polyurethane thermal insulation material is characterized by comprising the following steps:
step 1, preparing a flame-retardant heat-insulating material spinning solution: taking polyether polyol and a phosphate flame retardant, stirring, uniformly mixing, standing to completely eliminate bubbles, slowly adding ultrashort aromatic polysulphone fibers, stirring, ultrasonically treating until the ultrashort aromatic polysulphone fibers are uniformly dispersed, standing to completely eliminate bubbles, slowly adding isocyanate, standing to slowly and uniformly mix the isocyanate to obtain a flame-retardant heat-insulation material spinning solution;
step 2, electrostatic melt-blown flame-retardant heat-insulating material: pouring the flame-retardant heat-insulating material spinning solution obtained in the step (1) into a melt-blowing die head of electrostatic melt-blowing equipment, paving a nylon fiber receiving net under the melt-blowing die head, spraying a fiber bundle from a spinneret orifice by the flame-retardant heat-insulating material spinning solution obtained in the step (1) under the action of high-voltage direct current and high-pressure air, forming a layer of uniform and fluffy polyurethane fiber film on the surface of the nylon fiber receiving net after melt-blowing is finished, and drying the polyurethane fiber film;
step 3, preparing electromagnetic shielding electrostatic spinning solution: mixing polyvinylidene fluoride and DMF/acetone, stirring, and slowly adding Ti3C2MXenes, stirred, then sonicated to Ti3C2MXenes is dispersed uniformly and kept stand to obtain electromagnetic shielding electrostatic spinning solution;
step 4, electrostatic spinning electromagnetic shielding flame-retardant heat-insulating material: injecting the electromagnetic shielding electrostatic spinning solution obtained in the step 3 into electrostatic spinning needle tube equipment, paving the polyurethane fiber membrane obtained in the step 2 on an electrostatic spinning aluminum foil receiver, spraying a fiber bundle from an electrostatic spinning head by the electromagnetic shielding electrostatic spinning solution obtained in the step 3 under the action of direct-current voltage, forming a black polyurethane fiber membrane on the electrostatic spinning aluminum foil receiver after electrostatic spinning is finished, and drying the black polyurethane fiber membrane to obtain the MXenes/polyurethane heat-insulating material.
2. The preparation method of the MXenes/polyurethane thermal insulation material as claimed in claim 1, wherein the mass ratio of the polyether polyol, the phosphate ester flame retardant and the isocyanate in the step 1 is 15:3: 5-15, and the ultrashort polysulfonamide fiber is ultrashort polysulfonamide fiber with the mass fraction of 0-7.5 wt%.
3. The preparation method of the MXenes/polyurethane thermal insulation material as claimed in claim 1, wherein the stirring speed of the polyether polyol and the phosphate ester flame retardant in the step 1 is 1000-1200 rpm/min, and the stirring time is 10-15 min; adding the ultrashort polysulfonamide fibers, stirring at the rotating speed of 800-1200 rpm/min for 30-60 min.
4. The preparation method of the MXenes/polyurethane thermal insulation material according to claim 1, wherein in the step 2, the high-voltage direct current voltage is 38-40 KV, the pressure of high-pressure air is 0.05-0.12 MPa, the temperature of the high-pressure air is 23-26 ℃, the humidity of the high-pressure air is 30-40%, the distance between the tip of a spinneret of a melt-blowing die head and a nylon fiber receiving net is 800-1000 mm, the diameter of a spinneret hole is 0.4mm, the melt-blowing time is 40-100 minutes, the drying temperature is 60-70 ℃, and the drying time is 4-6 hours.
5. The method for preparing MXenes/polyurethane thermal insulation material according to claim 1, wherein polyvinylidene fluoride, DMF/acetone mixed solution and Ti in the step 33C2MXenes mass ratio 5.6:14.4:1, DMF to acetone volume ratio 7: 3.
6. The preparation method of the MXenes/polyurethane thermal insulation material as claimed in claim 1, wherein the stirring temperature of the mixed solution of polyvinylidene fluoride and DMF/acetone in the step 3 is 45-55 ℃, the stirring speed is 20-25 rpm/min, and the stirring time is 0.5-1 h; adding Ti3C2The rotation speed of MXenes stirring is 20-25 rpm/min, and the stirring time is 30-40And standing for 30-60 min.
7. The preparation method of the MXenes/polyurethane thermal insulation material as claimed in claim 1, wherein the distance between the tip of the electrostatic spinning head of the electrostatic spinning needle tube equipment and the electrostatic spinning aluminum foil receiver in the step 4 is 160-200 mm, the direct current voltage is 25-32 KV, the temperature is 23-26 ℃, the humidity is 30-40%, the drying temperature is 60-70 ℃, and the drying time is 2-4 h.
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| US20030148693A1 (en) * | 2001-07-19 | 2003-08-07 | Erb David F. | Thermal and acoustic insulation fabric |
| AU2003903431A0 (en) * | 2003-07-03 | 2003-07-17 | Commonwealth Scientific And Industrial Research Organisation | Electroconductive textiles |
| WO2005010262A1 (en) * | 2003-07-28 | 2005-02-03 | Toyo Boseki Kabushiki Kaisha | Reinforcing material for polyurethane foam molded article, cushioning material for seat, and seat |
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| CN105147356B (en) * | 2015-09-21 | 2017-09-12 | 青岛理工大学 | Cold grinding head in a kind of electrostatic atomization |
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| CN107660114A (en) * | 2017-09-08 | 2018-02-02 | 西安工程大学 | A kind of preparation method of molybdenum disulfide/MXene lamellar composite absorbing materials |
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| CN109576905B (en) * | 2018-12-05 | 2023-07-07 | 河北工业大学 | MXene-based flexible polyurethane fiber membrane strain sensor |
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