CN115259829A - Nano heat-insulating material and preparation method thereof - Google Patents

Nano heat-insulating material and preparation method thereof Download PDF

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CN115259829A
CN115259829A CN202210963315.0A CN202210963315A CN115259829A CN 115259829 A CN115259829 A CN 115259829A CN 202210963315 A CN202210963315 A CN 202210963315A CN 115259829 A CN115259829 A CN 115259829A
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nano
carbon fiber
pore
fiber
doped carbon
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韩福梅
向文艺
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Weihe Xinyuan Nanotechnology Suzhou Co ltd
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Weihe Xinyuan Nanotechnology Suzhou Co ltd
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    • C04B30/02—Compositions for artificial stone, not containing binders containing fibrous materials
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B14/00—Use of inorganic materials as fillers, e.g. pigments, for mortars, concrete or artificial stone; Treatment of inorganic materials specially adapted to enhance their filling properties in mortars, concrete or artificial stone
    • C04B14/38—Fibrous materials; Whiskers
    • C04B14/386—Carbon
    • C—CHEMISTRY; METALLURGY
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    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B14/00—Use of inorganic materials as fillers, e.g. pigments, for mortars, concrete or artificial stone; Treatment of inorganic materials specially adapted to enhance their filling properties in mortars, concrete or artificial stone
    • C04B14/38—Fibrous materials; Whiskers
    • C04B14/46—Rock wool ; Ceramic or silicate fibres
    • C04B14/4618—Oxides
    • C04B14/4625—Alumina
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    • C04B18/00—Use of agglomerated or waste materials or refuse as fillers for mortars, concrete or artificial stone; Treatment of agglomerated or waste materials or refuse, specially adapted to enhance their filling properties in mortars, concrete or artificial stone
    • C04B18/04—Waste materials; Refuse
    • C04B18/14—Waste materials; Refuse from metallurgical processes
    • C04B18/146—Silica fume
    • 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
    • D01F1/10—Other agents for modifying properties
    • 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
    • D01F6/94—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 other polycondensation products
    • 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
    • D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
    • D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
    • D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
    • D01F9/14—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments
    • D01F9/20—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products
    • D01F9/21—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products from macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D01F9/22—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products from macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds from polyacrylonitriles
    • 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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    • C04B2201/00—Mortars, concrete or artificial stone characterised by specific physical values
    • C04B2201/50—Mortars, concrete or artificial stone characterised by specific physical values for the mechanical strength
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W30/00—Technologies for solid waste management
    • Y02W30/50—Reuse, recycling or recovery technologies
    • Y02W30/91—Use of waste materials as fillers for mortars or concrete

Abstract

The invention provides a nano heat insulation material and a preparation method thereof, wherein the nano heat insulation material comprises the following components of 3-9% of a reinforced fiber membrane, 5-10% of nano-pore silicon-doped carbon fiber, 5-10% of an opacifier and the balance of modified silica fume with the particle size of 10-100 nm; wherein, the structure of the nano-pore silicon-doped carbon fiber is a spiral structure. The preparation method comprises the following steps: taking the reinforced fiber, the modified silica fume, the opacifier and the nano-pore silicon-doped carbon fiber, and placing the reinforced fiber, the modified silica fume, the opacifier and the nano-pore silicon-doped carbon fiber in a high-speed stirrer to be uniformly mixed; and (5) carrying out dry pressing to obtain a sample, and drying in an oven. The invention provides a nano heat insulation material and a preparation method thereof, which are characterized in that on the premise of not influencing or even improving the heat insulation effect, silica fume is used as a matrix raw material, and a reinforced fiber film and nano-pore silicon-doped carbon fiber are used as a reinforcement body, so that the nano heat insulation material with good heat insulation performance, high heat insulation performance under high temperature and good mechanical property is obtained.

Description

Nano heat-insulating material and preparation method thereof
Technical Field
The invention belongs to the field of composite functional materials, and particularly relates to a nanometer heat-insulating material and a preparation method thereof.
Background
Energy conservation is a long-term development strategy of sustainable development in China, and development of environment-friendly heat insulation materials by adopting new technology and new process is the most effective and most economical energy-saving measure. The nanometer heat insulating material is one kind of efficient heat insulating material developed in two years and developed based on the excellent heat insulating performance of nanometer pore material, and has SiO as main component 2 And the like. The existing nanometer heat insulating materials on the market have higher cost, and the main reason is that the used raw materials are expensive. Therefore, the application takes the silicon micropowder as a main raw material, and the silicon micropowder (known as 'silica fume') is amorphous and powdery silicon dioxide which is obtained by oxidizing silicon steam discharged from a flue during alloy smelting and collecting the oxidized silicon steam by a specially designed dust collector, and belongs to industrial waste. The average grain size of the micro silicon powder is 0.1-0.15 μm, which is one hundredth of the average grain size of cement, and the micro silicon powder has extremely strong surface activity. Meanwhile, the mechanical property of the pure silica fume heat-insulating material is poor, so that the application of the silica fume heat-insulating material in various aspects is limited. Therefore, it is necessary to add some materials for compounding to obtain a heat insulating material with good heat insulating performance and good mechanical properties.
Disclosure of Invention
The technical problem to be solved is as follows: aiming at the problems that the mechanical property of the existing heat insulation nano material is poor and the application of the existing heat insulation nano material in various aspects is limited, the invention aims to provide a nano heat insulation material and a preparation method thereof.
The technical scheme is as follows: a nanometer heat insulation material comprises the following components in percentage by weight: 3-9% of a reinforced fiber membrane, 5-10% of nano-pore silicon-doped carbon fiber, 5-10% of an opacifier and the balance of modified silica fume with the particle size of 10-100 nm; wherein, the structure of the nano-pore silicon-doped carbon fiber is a spiral structure.
Preferably, the diameter of the spiral structure is 0.1-0.5mm, and the height is 1-2mm.
Preferably, the pore diameter of the nanopore silicon-doped carbon fiber is less than or equal to 50nm.
Preferably, the reinforced fiber membrane is an ordered quartz fiber membrane, the pore diameter of pores is less than or equal to 50nm, and the diameter of quartz fibers is 400nm.
Preferably, the preparation method of the ordered quartz fiber membrane comprises the following steps:
1) Taking 100 parts of silica sol with the particle size of 5-100nm and the solid content of 20-40wt.%, and adjusting the pH value to 4;
2) Adding 100 parts of polyethylene glycol and 1 part of alumina sol, mixing and stirring uniformly, standing and defoaming to obtain a spinning solution;
3) Adding the spinning solution into an injector of an electrostatic spinning device, and applying direct current high voltage to spray the solution;
4) Receiving the ordered fiber by a rotating winding drum, wherein the voltage is 12kV, the flow is 0.5mL/h, the distance between a needle head and the winding drum is 20cm, and the rotating speed of an electric spindle is 8000r/min;
5) Drying the ordered fiber, calcining in a kiln, slowly heating to 1300 ℃ after 25 hours, and carrying out heat preservation and calcination for 8 hours;
6) Taking out and crushing to obtain ordered quartz fiber films with the length and the width of 1mm multiplied by 1mm respectively.
Preferably, the preparation method of the nano-pore silicon-doped carbon fiber comprises the following steps:
(1) Preparing polyacrylonitrile solution with the content of 6-10wt.% by adopting N' N-dimethylformamide, standing and carrying out vacuum defoaming to obtain spinning solution;
(2) Placing in an electrostatic spinning device, receiving by a receiving plate, and fixing a spiral calcium carbonate model on the receiving plate, wherein the spinning voltage is 14-20kV, and the spinning distance is 12-20cm;
(3) Taking down and sintering the polyacrylonitrile fiber with the nano-pore spiral structure;
(4) Washing with dilute hydrochloric acid to obtain the carbon fiber with the nano-pore spiral structure;
(5) And (3) soaking the carbon fiber with the nano-pore spiral structure in tetraethoxysilane with the concentration, taking out and drying to obtain the nano-pore carbon fiber.
Preferably, the sintering method comprises the following steps: pre-oxidizing at 250-260 deg.c for 1.5-2.5 hr, and carbonizing at 800-1100 deg.c for 1 hr.
Preferably, the preparation method of the modified micro silicon powder comprises the following steps: dispersing the micro silicon powder in water uniformly, adding dopamine hydrochloride, adjusting the pH value to 7.5-10.5, reacting, washing and drying the product to obtain the product.
Preferably, the micro silicon powder is recovered by an alloy electric furnace dust removal system, and the specific surface area is 15-27m 2 The purity is more than or equal to 99 percent per gram. The preparation method of the nanometer heat-insulating material comprises the following steps:
(1) Taking the reinforced fiber, the modified silica fume with the particle size of 10-100nm, the opacifier and the nano-pore silicon-doped carbon fiber, placing the materials in a high-speed stirrer, and mixing the materials at the rotating speed of 500r/min for 10min;
(2) Mixing materials at a rotating speed of 1500r/min for 15min to be uniformly mixed;
(3) The sample was obtained by dry press molding under a pressure of 0.1MPa, and the sample was dried in an oven at 110 ℃ for 12 hours.
Has the beneficial effects that:
1. the invention adopts the micro silicon powder as the main raw material, the micro silicon powder is recovered by adopting an alloy electric furnace dust removal system, and the invention belongs to industrial waste 2 The obtained micro silicon powder belongs to waste recycling, has low cost and simultaneously has excellent heat insulation effect.
2. After the micro silicon powder is treated by dopamine hydrochloride, the dispersion can be effectively promoted, and the agglomeration is prevented.
3. The ordered quartz fiber membrane is prepared by electrostatic spinning, has nano pores, and can enhance the mechanical property and reduce the influence on the heat-insulating property to the maximum extent. The ordered quartz fiber film is of a three-dimensional structure, so that load can be effectively transferred from the micro silicon powder substrate to the reinforcement fiber, the bonding performance between the substrate and the reinforcement is improved, and the mechanical strength is further improved. In addition, at high temperature, the quartz fiber film can also improve the heat insulation performance of the material under high temperature conditions due to the characteristics of the quartz fiber.
4. The invention adopts the nano-pore silicon-doped carbon fiber, the structure is spiral, the three-dimensional structure of the spiral nano-pore silicon-doped carbon fiber not only plays a role of uniformly dispersing raw materials in raw material mixing and preventing agglomeration, but also has a special three-dimensional structure, the fracture behavior shows the step-by-step fracture of a typical three-dimensional structure, and the fracture toughness is also greatly improved compared with that of a two-dimensional structure.
5. In the process of compression molding of the material, the contact area of the micro silicon powder, the reinforced fiber film and the nano-pore silicon-doped carbon fiber is remarkably increased and combined together, particularly the reinforced fiber film and the nano-pore silicon-doped carbon fiber are of three-dimensional structures, particularly the nano-pore silicon-doped carbon fiber is spiral, so that the reinforced fiber film and the nano-pore silicon-doped carbon fiber can fully transmit and disperse stress load when a sample is pressed, and the compressive strength of the material is improved.
Detailed Description
Example 1
A nanometer heat-insulating material comprises the following components in percentage by weight: 3% of reinforced fiber membrane, 5% of nano-pore silicon-doped carbon fiber and 5% of opacifier TiO 2 The balance of modified micro silicon powder with the particle size of 10-100 nm; wherein, the first and the second end of the pipe are connected with each other,
the structure of the nano-pore silicon-doped carbon fiber is a spiral structure, the diameter of the spiral structure is 0.1mm, and the height of the spiral structure is 1mm; the pore diameter of the nanometer pore silicon-doped carbon fiber is less than or equal to 50nm;
the preparation method of the nano-pore silicon-doped carbon fiber comprises the following steps:
(1) Preparing polyacrylonitrile solution with the content of 6wt.% by adopting N' N-dimethylformamide, standing and defoaming in vacuum to obtain spinning solution;
(2) Placing the mixture in an electrostatic spinning device, receiving by a receiving plate, and fixing a spiral-structure calcium carbonate model on the receiving plate, wherein the spinning voltage is 14kV, and the spinning distance is 15cm;
(3) Taking down and sintering the polyacrylonitrile fiber with the nano-pore spiral structure, wherein the sintering method comprises the following steps: pre-oxidizing at 250 deg.c for 1.5, and carbonizing at 800 deg.c for 1 hr;
(4) Washing with dilute hydrochloric acid to obtain the carbon fiber with the nano-pore spiral structure;
(5) And (3) soaking the carbon fiber with the nano-pore spiral structure in tetraethoxysilane with the concentration, taking out and drying to obtain the nano-pore carbon fiber.
The reinforced fiber membrane is an ordered quartz fiber membrane, the pore diameter of pores is less than or equal to 50nm, and the diameter of quartz fibers is 400nm;
the preparation method of the ordered quartz fiber membrane comprises the following steps:
1) Taking 100 parts of silica sol with the particle size of 5-100nm and the solid content of 30wt.%, and adjusting the pH value to 4;
2) Adding 100 parts of polyethylene glycol and 1 part of alumina sol, mixing and stirring uniformly, standing and defoaming to obtain a spinning solution;
3) Adding the spinning solution into an injector of an electrostatic spinning device, and applying direct current high voltage to spray the solution;
4) Receiving the ordered fiber by a rotating winding drum, wherein the voltage is 12kV, the flow is 0.5mL/h, the distance between a needle head and the winding drum is 20cm, and the rotating speed of an electric spindle is 8000r/min;
5) Drying the ordered fibers, calcining in a kiln, slowly heating to 1300 ℃ within 25h, and carrying out heat preservation and calcination for 8h;
6) Taking out and crushing to obtain ordered quartz fiber films with the length and the width of 1mm multiplied by 1mm respectively.
The preparation method of the modified micro silicon powder comprises the following steps: dispersing the silica fume in water uniformly, adding dopamine hydrochloride, adjusting pH value to 8, reacting, washing and drying the product to obtain the silica fume, wherein the silica fume is recovered by an alloy electric furnace dust removal system, and the specific surface area is 15-27m 2 The purity is more than or equal to 99 percent per gram.
The preparation method of the nanometer heat-insulating material comprises the following steps:
(1) Taking the reinforced fiber, the modified silica fume with the particle size of 10-100nm, the opacifier and the nano-pore silicon-doped carbon fiber, placing the materials in a high-speed stirrer, and mixing the materials at the rotating speed of 500r/min for 10min;
(2) Mixing materials at a rotating speed of 1500r/min for 15min to be uniformly mixed;
(3) The sample is prepared by dry pressing under the pressure of 0.1MPa, and the sample is dried in an oven at the temperature of 110 ℃ for 12 hours.
The material thickness was 10mm.
Example 2
A nanometer heat-insulating material comprises the following components in percentage by weight: 5% of reinforced fiber membrane and 5% of nano-porous admixtureSilicon carbon fiber and 5% of opacifier TiO 2 The balance of modified micro silicon powder with the particle size of 10-100 nm; wherein the content of the first and second substances,
the structure of the nano-pore silicon-doped carbon fiber is a spiral structure, the diameter of the spiral structure is 0.1mm, and the height of the spiral structure is 1mm; the pore diameter of the nanometer pore silicon-doped carbon fiber is less than or equal to 50nm;
the preparation method of the nano-pore silicon-doped carbon fiber comprises the following steps:
(1) Preparing polyacrylonitrile solution with the content of 6wt.% by adopting N' N-dimethylformamide, standing and defoaming in vacuum to obtain spinning solution;
(2) Placing the fiber into an electrostatic spinning device, receiving by a receiving plate, and fixing a spiral calcium carbonate model on the receiving plate, wherein the spinning voltage is 14kV, and the spinning distance is 15cm;
(3) Taking down and sintering the polyacrylonitrile fiber with the nano-pore spiral structure, wherein the sintering method comprises the following steps: pre-oxidizing at 250 deg.c for 1.5, and carbonizing at 800 deg.c for 1 hr;
(4) Washing with dilute hydrochloric acid to obtain the carbon fiber with the nano-pore spiral structure;
(5) And (3) soaking the carbon fiber with the nano-pore spiral structure in tetraethoxysilane with the concentration, taking out and drying to obtain the carbon fiber.
The reinforced fiber membrane is an ordered quartz fiber membrane, the pore diameter of pores is less than or equal to 50nm, and the diameter of quartz fibers is 400nm;
the preparation method of the ordered quartz fiber membrane comprises the following steps:
1) Taking 100 parts of silica sol with the particle size of 5-100nm and the solid content of 30wt.%, and adjusting the pH value to 4;
2) Adding 100 parts of polyethylene glycol and 1 part of alumina sol, mixing and stirring uniformly, standing and defoaming to obtain a spinning solution;
3) Adding the spinning solution into an injector of an electrostatic spinning device, and applying direct current high voltage to spray the solution;
4) Receiving the ordered fiber by a rotating winding drum, wherein the voltage is 12kV, the flow is 0.5mL/h, the distance between a needle head and the winding drum is 20cm, and the rotating speed of an electric spindle is 8000r/min;
5) Drying the ordered fiber, calcining in a kiln, slowly heating to 1300 ℃ after 25 hours, and carrying out heat preservation and calcination for 8 hours;
6) Taking out and crushing to obtain ordered quartz fiber films with the length and the width of 1mm multiplied by 1mm respectively.
The preparation method of the modified micro silicon powder comprises the following steps: dispersing micro silicon powder in water uniformly, adding dopamine hydrochloride, adjusting pH value to 8, reacting, washing and drying the product to obtain the product, wherein the micro silicon powder is recovered by an alloy electric furnace dust removal system, and the specific surface area is 15-27m 2 The purity is more than or equal to 99 percent per gram.
The preparation method of the nanometer heat-insulating material comprises the following steps:
(1) Taking the reinforced fiber, the modified silica fume with the particle size of 10-100nm, the opacifier and the nano-pore silicon-doped carbon fiber, placing the materials in a high-speed stirrer, and mixing the materials at the rotating speed of 500r/min for 10min;
(2) Mixing materials at a rotation speed of 1500r/min for 15min to be uniformly mixed;
(3) The sample is prepared by dry pressing under the pressure of 0.1MPa, and the sample is dried in an oven at the temperature of 110 ℃ for 12 hours.
The material thickness was 10mm.
Example 3
A nanometer heat-insulating material comprises the following components in percentage by weight: 7% of reinforced fiber membrane, 5% of nano-pore silicon-doped carbon fiber and 5% of opacifier TiO 2 The balance of modified micro silicon powder with the particle size of 10-100 nm; wherein the content of the first and second substances,
the structure of the nano-pore silicon-doped carbon fiber is a spiral structure, the diameter of the spiral structure is 0.1mm, and the height of the spiral structure is 1mm; the pore diameter of the nanometer pores of the nanometer pore silicon-doped carbon fiber is less than or equal to 50nm;
the preparation method of the nano-pore silicon-doped carbon fiber comprises the following steps:
(1) Preparing polyacrylonitrile solution with the content of 6wt.% by adopting N' N-dimethylformamide, standing and defoaming in vacuum to obtain spinning solution;
(2) Placing the mixture in an electrostatic spinning device, receiving by a receiving plate, and fixing a spiral-structure calcium carbonate model on the receiving plate, wherein the spinning voltage is 14kV, and the spinning distance is 15cm;
(3) Taking down and sintering the polyacrylonitrile fiber with the nano-pore spiral structure, wherein the sintering method comprises the following steps: pre-oxidizing at 250 deg.c for 1.5, and carbonizing at 800 deg.c for 1 hr;
(4) Washing with dilute hydrochloric acid to obtain the carbon fiber with the nano-pore spiral structure;
(5) And (3) soaking the carbon fiber with the nano-pore spiral structure in tetraethoxysilane with the concentration, taking out and drying to obtain the nano-pore carbon fiber.
The reinforced fiber membrane is an ordered quartz fiber membrane, the pore diameter of pores is less than or equal to 50nm, and the diameter of quartz fibers is 400nm;
the preparation method of the ordered quartz fiber membrane comprises the following steps:
1) Taking 100 parts of silica sol with the particle size of 5-100nm and the solid content of 30wt.%, and adjusting the pH value to 4;
2) Adding 100 parts of polyethylene glycol and 1 part of alumina sol, mixing and stirring uniformly, standing and defoaming to obtain a spinning solution;
3) Adding the spinning solution into an injector of an electrostatic spinning device, and applying direct current high voltage to spray the solution;
4) Receiving the ordered fiber by a rotating winding drum, wherein the voltage is 12kV, the flow is 0.5mL/h, the distance between a needle head and the winding drum is 20cm, and the rotating speed of an electric spindle is 8000r/min;
5) Drying the ordered fiber, calcining in a kiln, slowly heating to 1300 ℃ after 25 hours, and carrying out heat preservation and calcination for 8 hours;
6) Taking out and crushing to obtain ordered quartz fiber films with the length and the width of 1mm multiplied by 1mm respectively.
The preparation method of the modified micro silicon powder comprises the following steps: dispersing the silica fume in water uniformly, adding dopamine hydrochloride, adjusting pH value to 8, reacting, washing and drying the product to obtain the silica fume, wherein the silica fume is recovered by an alloy electric furnace dust removal system, and the specific surface area is 15-27m 2 The purity is more than or equal to 99 percent per gram.
The preparation method of the nanometer heat-insulating material comprises the following steps:
(1) Taking the reinforced fiber, the modified silica fume with the particle size of 10-100nm, the opacifier and the nano-pore silicon-doped carbon fiber, placing the materials in a high-speed stirrer, and mixing the materials at the rotating speed of 500r/min for 10min;
(2) Mixing materials at a rotating speed of 1500r/min for 15min to be uniformly mixed;
(3) The sample is prepared by dry pressing under the pressure of 0.1MPa, and the sample is dried in an oven at the temperature of 110 ℃ for 12 hours.
The material thickness was 10mm.
Example 4
A nanometer heat-insulating material comprises the following components in percentage by weight: 9% of reinforced fiber film, 5% of nano-pore silicon-doped carbon fiber and 5% of opacifier TiO 2 The balance of modified micro silicon powder with the particle size of 10-100 nm; wherein the content of the first and second substances,
the structure of the nano-pore silicon-doped carbon fiber is a spiral structure, the diameter of the spiral structure is 0.1mm, and the height of the spiral structure is 1mm; the pore diameter of the nanometer pore silicon-doped carbon fiber is less than or equal to 50nm;
the preparation method of the nano-pore silicon-doped carbon fiber comprises the following steps:
(1) Preparing polyacrylonitrile solution with the content of 6wt.% by adopting N' N-dimethylformamide, standing and defoaming in vacuum to obtain spinning solution;
(2) Placing the fiber into an electrostatic spinning device, receiving by a receiving plate, and fixing a spiral calcium carbonate model on the receiving plate, wherein the spinning voltage is 14kV, and the spinning distance is 15cm;
(3) Taking down and sintering the polyacrylonitrile fiber with the nano-pore spiral structure, wherein the sintering method comprises the following steps: pre-oxidizing at 250 deg.c for 1.5, and carbonizing at 800 deg.c for 1 hr;
(4) Washing with dilute hydrochloric acid to obtain the carbon fiber with the nano-pore spiral structure;
(5) And (3) soaking the carbon fiber with the nano-pore spiral structure in tetraethoxysilane with the concentration, taking out and drying to obtain the nano-pore carbon fiber.
The reinforced fiber membrane is an ordered quartz fiber membrane, the pore diameter of pores is less than or equal to 50nm, and the diameter of quartz fibers is 400nm;
the preparation method of the ordered quartz fiber membrane comprises the following steps:
1) Taking 100 parts of silica sol with the particle size of 5-100nm and the solid content of 30wt.%, and adjusting the pH value to 4;
2) Adding 100 parts of polyethylene glycol and 1 part of alumina sol, mixing and stirring uniformly, standing and defoaming to obtain a spinning solution;
3) Adding the spinning solution into an injector of an electrostatic spinning device, and applying direct current high voltage to spray the solution;
4) Receiving the ordered fiber by a rotating winding drum, wherein the voltage is 12kV, the flow is 0.5mL/h, the distance between a needle head and the winding drum is 20cm, and the rotating speed of an electric spindle is 8000r/min;
5) Drying the ordered fibers, calcining in a kiln, slowly heating to 1300 ℃ within 25h, and carrying out heat preservation and calcination for 8h;
6) Taking out and crushing to obtain ordered quartz fiber films with the length and the width of 1mm multiplied by 1mm respectively.
The preparation method of the modified micro silicon powder comprises the following steps: dispersing the silica fume in water uniformly, adding dopamine hydrochloride, adjusting pH value to 8, reacting, washing and drying the product to obtain the silica fume, wherein the silica fume is recovered by an alloy electric furnace dust removal system, and the specific surface area is 15-27m 2 The purity is more than or equal to 99 percent per gram.
The preparation method of the nano heat insulation material comprises the following steps:
(1) Taking the reinforced fiber, the modified silica fume with the particle size of 10-100nm, the opacifier and the nano-pore silicon-doped carbon fiber, placing the materials in a high-speed stirrer, and mixing the materials at the rotating speed of 500r/min for 10min;
(2) Mixing materials at a rotating speed of 1500r/min for 15min to be uniformly mixed;
(3) The sample is prepared by dry pressing under the pressure of 0.1MPa, and the sample is dried in an oven at the temperature of 110 ℃ for 12 hours.
The material thickness was 10mm.
Example 5
A nanometer heat insulation material comprises the following components in percentage by weight: 7% of reinforced fiber membrane, 8% of nano-pore silicon-doped carbon fiber and 8% of opacifier TiO 2 The balance of modified micro silicon powder with the particle size of 10-100 nm; wherein the content of the first and second substances,
the structure of the nano-pore silicon-doped carbon fiber is a spiral structure, the diameter of the spiral structure is 0.1mm, and the height of the spiral structure is 1mm; the pore diameter of the nanometer pore silicon-doped carbon fiber is less than or equal to 50nm;
the preparation method of the nano-pore silicon-doped carbon fiber comprises the following steps:
(1) Preparing polyacrylonitrile solution with the content of 6wt.% by adopting N' N-dimethylformamide, standing and defoaming in vacuum to obtain spinning solution;
(2) Placing the fiber into an electrostatic spinning device, receiving by a receiving plate, and fixing a spiral calcium carbonate model on the receiving plate, wherein the spinning voltage is 14kV, and the spinning distance is 15cm;
(3) Taking down and sintering the polyacrylonitrile fiber with the nano-pore spiral structure, wherein the sintering method comprises the following steps: pre-oxidizing at 250 deg.c for 1.5, and carbonizing at 800 deg.c for 1 hr;
(4) Washing with dilute hydrochloric acid to obtain the carbon fiber with the nano-pore spiral structure;
(5) And (3) soaking the carbon fiber with the nano-pore spiral structure in tetraethoxysilane with the concentration, taking out and drying to obtain the nano-pore carbon fiber.
The reinforced fiber membrane is an ordered quartz fiber membrane, the pore diameter of pores is less than or equal to 50nm, and the diameter of quartz fibers is 400nm;
the preparation method of the ordered quartz fiber membrane comprises the following steps:
1) Taking 100 parts of silica sol with the particle size of 5-100nm and the solid content of 30wt.%, and adjusting the pH value to 4;
2) Adding 100 parts of polyethylene glycol and 1 part of alumina sol, mixing and stirring uniformly, standing and defoaming to obtain a spinning solution;
3) Adding the spinning solution into an injector of an electrostatic spinning device, and applying direct current high voltage to spray the solution;
4) Receiving the ordered fiber by a rotating winding drum, wherein the voltage is 12kV, the flow rate is 0.5mL/h, the distance between a needle head and the winding drum is 20cm, and the rotating speed of an electric main shaft is 8000r/min;
5) Drying the ordered fiber, calcining in a kiln, slowly heating to 1300 ℃ after 25 hours, and carrying out heat preservation and calcination for 8 hours;
6) Taking out and crushing to obtain ordered quartz fiber films with the length and the width of 1mm multiplied by 1mm respectively.
The preparation method of the modified micro silicon powder comprises the following steps: dispersing micro silicon powder in water uniformly, adding dopamine hydrochloride, adjusting pH value to 8, reacting, washing and drying the product to obtain the product, wherein the micro silicon powder is recovered by an alloy electric furnace dust removal system, and the specific surface area is 15-27m 2 The purity is more than or equal to 99 percent per gram.
The preparation method of the nano heat insulation material comprises the following steps:
(1) Taking the reinforced fiber, the modified silica fume with the particle size of 10-100nm, the opacifier and the nano-pore silicon-doped carbon fiber, placing the materials in a high-speed stirrer, and mixing the materials at the rotating speed of 500r/min for 10min;
(2) Mixing materials at a rotating speed of 1500r/min for 15min to be uniformly mixed;
(3) The sample is prepared by dry pressing under the pressure of 0.1MPa, and the sample is dried in an oven at the temperature of 110 ℃ for 12 hours.
4 kinds of materials with the thickness are respectively prepared, wherein the thickness of the material 5A is 5mm, the thickness of the material 5B is 10mm, the thickness of the material 5C is 30mm, and the thickness of the material 5D is 50mm.
Example 6
A nanometer heat-insulating material comprises the following components in percentage by weight: 7% of reinforced fiber membrane, 10% of nano-pore silicon-doped carbon fiber and 8% of opacifier TiO 2 The balance of modified micro silicon powder with the particle size of 10-100 nm; wherein, the first and the second end of the pipe are connected with each other,
the structure of the nano-pore silicon-doped carbon fiber is a spiral structure, the diameter of the spiral structure is 0.1mm, and the height of the spiral structure is 1mm; the pore diameter of the nanometer pore silicon-doped carbon fiber is less than or equal to 50nm;
the preparation method of the nano-pore silicon-doped carbon fiber comprises the following steps:
(1) Preparing polyacrylonitrile solution with the content of 6wt.% by adopting N', N-dimethylformamide, standing, and performing vacuum defoaming to obtain spinning solution;
(2) Placing the mixture in an electrostatic spinning device, receiving by a receiving plate, and fixing a spiral-structure calcium carbonate model on the receiving plate, wherein the spinning voltage is 14kV, and the spinning distance is 15cm;
(3) Taking down and sintering the polyacrylonitrile fiber with the nano-pore spiral structure, wherein the sintering method comprises the following steps: pre-oxidizing at 250 deg.c for 1.5, and carbonizing at 800 deg.c for 1 hr;
(4) Washing with dilute hydrochloric acid to obtain the carbon fiber with the nano-pore spiral structure;
(5) And (3) soaking the carbon fiber with the nano-pore spiral structure in tetraethoxysilane with the concentration, taking out and drying to obtain the carbon fiber.
The reinforced fiber membrane is an ordered quartz fiber membrane, the pore diameter of pores is less than or equal to 50nm, and the diameter of quartz fibers is 400nm;
the preparation method of the ordered quartz fiber membrane comprises the following steps:
1) Taking 100 parts of silica sol with the particle size of 5-100nm and the solid content of 30wt.%, and adjusting the pH value to 4;
2) Adding 100 parts of polyethylene glycol and 1 part of alumina sol, mixing and stirring uniformly, standing and defoaming to obtain a spinning solution;
3) Adding the spinning solution into an injector of an electrostatic spinning device, and applying direct current high voltage to spray the solution;
4) Receiving the ordered fiber by a rotating winding drum, wherein the voltage is 12kV, the flow is 0.5mL/h, the distance between a needle head and the winding drum is 20cm, and the rotating speed of an electric spindle is 8000r/min;
5) Drying the ordered fiber, calcining in a kiln, slowly heating to 1300 ℃ after 25 hours, and carrying out heat preservation and calcination for 8 hours;
6) Taking out and crushing to obtain ordered quartz fiber films with the length and the width of 1mm multiplied by 1mm respectively.
The preparation method of the modified micro silicon powder comprises the following steps: dispersing the silica fume in water uniformly, adding dopamine hydrochloride, adjusting pH value to 8, reacting, washing and drying the product to obtain the silica fume, wherein the silica fume is recovered by an alloy electric furnace dust removal system, and the specific surface area is 15-27m 2 The purity is more than or equal to 99 percent per gram.
The preparation method of the nanometer heat-insulating material comprises the following steps:
(1) Taking the reinforced fiber, the modified silica fume with the particle size of 10-100nm, the opacifier and the nano-pore silicon-doped carbon fiber, placing the materials in a high-speed stirrer, and mixing the materials at the rotating speed of 500r/min for 10min;
(2) Mixing materials at a rotating speed of 1500r/min for 15min to be uniformly mixed;
(3) The sample was obtained by dry press molding under a pressure of 0.1MPa, and the sample was dried in an oven at 110 ℃ for 12 hours.
The material thickness was 10mm.
Example 7
A nanometer heat insulation material comprises the following components in percentage by weight: 9% of reinforced fiber film, 10% of nano-pore silicon-doped carbon fiber and 10% of opacifier TiO 2 The balance of modified silica fume with the particle size of 10-100 nm; wherein the content of the first and second substances,
the structure of the nano-pore silicon-doped carbon fiber is a spiral structure, the diameter of the spiral structure is 0.5mm, and the height of the spiral structure is 2mm; the pore diameter of the nanometer pore silicon-doped carbon fiber is less than or equal to 50nm;
the preparation method of the nano-pore silicon-doped carbon fiber comprises the following steps:
(1) Preparing 10wt.% polyacrylonitrile solution by using N' N-dimethylformamide, standing and defoaming in vacuum to obtain spinning solution;
(2) Placing the fiber into an electrostatic spinning device, receiving by a receiving plate, and fixing a spiral calcium carbonate model on the receiving plate, wherein the spinning voltage is 20kV, and the spinning distance is 20cm;
(3) Taking down and sintering the polyacrylonitrile fiber with the nano-pore spiral structure, wherein the sintering method comprises the following steps: pre-oxidizing at 260 deg.c for 2.5 hr, and carbonizing at 1100 deg.c for 1 hr;
(4) Washing with dilute hydrochloric acid to obtain the carbon fiber with the nano-pore spiral structure;
(5) And (3) soaking the carbon fiber with the nano-pore spiral structure in tetraethoxysilane with the concentration, taking out and drying to obtain the carbon fiber.
The reinforced fiber membrane is an ordered quartz fiber membrane, the pore diameter of pores is less than or equal to 50nm, and the diameter of quartz fibers is 400nm;
the preparation method of the ordered quartz fiber membrane comprises the following steps:
1) Taking 100 parts of silica sol with the particle size of 5-100nm and the solid content of 40wt.%, and adjusting the pH value to 4;
2) Adding 100 parts of polyethylene glycol and 1 part of alumina sol, mixing and stirring uniformly, standing and defoaming to obtain a spinning solution;
3) Adding the spinning solution into an injector of an electrostatic spinning device, and applying direct current high voltage to spray the solution;
4) Receiving the ordered fiber by a rotating winding drum, wherein the voltage is 12kV, the flow is 0.5mL/h, the distance between a needle head and the winding drum is 20cm, and the rotating speed of an electric spindle is 8000r/min;
5) Drying the ordered fiber, calcining in a kiln, slowly heating to 1300 ℃ after 25 hours, and carrying out heat preservation and calcination for 8 hours;
6) Taking out and crushing to obtain ordered quartz fiber films with the length and the width of 1mm multiplied by 1mm respectively.
The preparation method of the modified micro silicon powder comprises the following steps: dispersing the silica fume in water uniformly, adding dopamine hydrochloride, adjusting the pH value to 7.5-10.5, reacting, washing and drying the product to obtain the silica fume, wherein the silica fume is recovered by an alloy electric furnace dust removal system, and the specific surface area is 15-27m 2 The purity is more than or equal to 99 percent per gram.
The preparation method of the nano heat insulation material comprises the following steps:
(1) Taking the reinforced fiber, the modified silica fume with the particle size of 10-100nm, the opacifier and the nano-pore silicon-doped carbon fiber, placing the materials in a high-speed stirrer, and mixing the materials at the rotating speed of 500r/min for 10min;
(2) Mixing materials at a rotation speed of 1500r/min for 15min to be uniformly mixed;
(3) The sample is prepared by dry pressing under the pressure of 0.1MPa, and the sample is dried in an oven at the temperature of 110 ℃ for 12 hours.
The material thickness was 10mm.
Comparative example 1
The comparative example is different from example 5 in that no reinforcing fiber membrane is added, and specifically the following are:
a nanometer heat-insulating material comprises the following components in percentage by weight: 8% of nano-pore silicon-doped carbon fiber and 8% of opacifier TiO 2 The balance of modified micro silicon powder with the particle size of 10-100 nm; wherein the content of the first and second substances,
the structure of the nano-pore silicon-doped carbon fiber is a spiral structure, the diameter of the spiral structure is 0.1mm, and the height of the spiral structure is 1mm; the pore diameter of the nanometer pores of the nanometer pore silicon-doped carbon fiber is less than or equal to 50nm;
the preparation method of the nano-pore silicon-doped carbon fiber comprises the following steps:
(1) Preparing polyacrylonitrile solution with the content of 6wt.% by adopting N' N-dimethylformamide, standing and defoaming in vacuum to obtain spinning solution;
(2) Placing the fiber into an electrostatic spinning device, receiving by a receiving plate, and fixing a spiral calcium carbonate model on the receiving plate, wherein the spinning voltage is 14kV, and the spinning distance is 15cm;
(3) Taking down and sintering the polyacrylonitrile fiber with the nano-pore spiral structure, wherein the sintering method comprises the following steps: pre-oxidizing at 250 deg.c for 1.5, and carbonizing at 800 deg.c for 1 hr;
(4) Washing with dilute hydrochloric acid to obtain the carbon fiber with the nano-pore spiral structure;
(5) And (3) soaking the carbon fiber with the nano-pore spiral structure in tetraethoxysilane with the concentration, taking out and drying to obtain the carbon fiber.
The preparation method of the modified micro silicon powder comprises the following steps: dispersing micro silicon powder in water uniformly, adding dopamine hydrochloride, adjusting pH value to 8, reacting, washing and drying the product to obtain the product, wherein the micro silicon powder is recovered by an alloy electric furnace dust removal system, and the specific surface area is 15-27m 2 The purity is more than or equal to 99 percent per gram.
The preparation method of the nanometer heat-insulating material comprises the following steps:
(1) Taking modified silica fume with the particle size of 10-100nm, an opacifier and nano-pore silicon-doped carbon fibers, placing the materials in a high-speed stirrer, and mixing the materials at the rotating speed of 500r/min for 10min;
(2) Mixing materials at a rotating speed of 1500r/min for 15min to be uniformly mixed;
(3) The sample was obtained by dry press molding under a pressure of 0.1MPa, and the sample was dried in an oven at 110 ℃ for 12 hours.
The material thickness was 10mm.
Comparative example 2
Compared with example 5, the difference of the comparative example is that the nano-pore silicon-doped carbon fiber is not added, and the specific steps are as follows:
a nanometer heat-insulating material comprises the following components in percentage by weight: 7% of reinforced fiber film and 8% of opacifier TiO 2 The balance of modified micro silicon powder with the particle size of 10-100 nm; wherein the content of the first and second substances,
the reinforced fiber membrane is an ordered quartz fiber membrane, the pore diameter of pores is less than or equal to 50nm, and the diameter of quartz fibers is 400nm;
the preparation method of the ordered quartz fiber membrane comprises the following steps:
1) Taking 100 parts of silica sol with the particle size of 5-100nm and the solid content of 30wt.%, and adjusting the pH value to 4;
2) Adding 100 parts of polyethylene glycol and 1 part of alumina sol, mixing and stirring uniformly, standing and defoaming to obtain a spinning solution;
3) Adding the spinning solution into an injector of an electrostatic spinning device, and applying direct current high voltage to spray the solution;
4) Receiving the ordered fiber by a rotating winding drum, wherein the voltage is 12kV, the flow is 0.5mL/h, the distance between a needle head and the winding drum is 20cm, and the rotating speed of an electric spindle is 8000r/min;
5) Drying the ordered fiber, calcining in a kiln, slowly heating to 1300 ℃ after 25 hours, and carrying out heat preservation and calcination for 8 hours;
6) Taking out and crushing to obtain ordered quartz fiber films with the length and the width of 1mm multiplied by 1mm respectively.
The preparation method of the modified micro silicon powder comprises the following steps: dispersing the micro silicon powder in water uniformly, adding dopamine hydrochloride, adjusting pH value to 8, reacting, washing and drying the product to obtain the product,wherein the micro silicon powder is recovered by an alloy electric furnace dust removal system, and the specific surface area is 15-27m 2 The purity is more than or equal to 99 percent per gram.
The preparation method of the nano heat insulation material comprises the following steps:
(1) Taking the reinforced fiber, the modified silica fume with the particle size of 10-100nm, the opacifier and the nano-pore silicon-doped carbon fiber, placing the materials in a high-speed stirrer, and mixing the materials at the rotating speed of 500r/min for 10min;
(2) Mixing materials at a rotation speed of 1500r/min for 15min to be uniformly mixed;
(3) The sample is prepared by dry pressing under the pressure of 0.1MPa, and the sample is dried in an oven at the temperature of 110 ℃ for 12 hours.
The material thickness was 10mm.
Comparative example 3
Compared with example 5, the difference of the comparative example is that the linear type nanometer hole silicon-doped carbon fiber bundle replaces the spiral nanometer hole silicon-doped carbon fiber, and the specific is as follows:
the diameter of the linear type nanopore silicon-doped carbon fiber bundle is 0.1mm, and the length of the linear type nanopore silicon-doped carbon fiber bundle is 1mm; the pore diameter of the nanometer pore silicon-doped carbon fiber is less than or equal to 50nm.
The material thickness was 10mm.
TABLE 1 temperature chart of each example
Figure BDA0003793942220000121
Table 2 temperature table of example 5 material
Figure BDA0003793942220000122
Figure BDA0003793942220000131
TABLE 3 mechanical Properties of the materials of the examples
Compressive strength MPa Bending strength MPa Fracture toughness MPa m 1/2
Example 1 5.29 85.2 1.19
Example 2 6.34 95.8 1.32
Example 3 7.17 102.3 1.51
Example 4 7.88 113.4 1.64
Example 5 (Material 5B) 7.93 114.6 1.67
Example 6 7.97 115.1 1.68
Example 7 8.01 115.7 1.69
Comparative example 1 3.83 88.2 1.42
Comparative example 2 4.12 76.3 1.28
Comparative example 3 6.76 101.6 1.49
It can be seen from table 1 that the addition of the reinforced fiber film has a certain influence on the heat insulation of the material, the influence within 300 ℃ is small, at this time, the heat conduction is mainly performed, after 600 ℃, the infrared heat radiation plays a leading role in the heat conduction, the addition of the reinforced fiber film causes the heat insulation to be reduced, but the influence on the heat insulation is greatly reduced because the reinforced fiber film also has nano pores. In addition, at high temperatures, the reinforced fiber membranes can also improve the thermal insulation properties of the material at high temperatures. The addition of the spiral nano-pore silicon-doped carbon fiber has almost no influence on the heat insulation performance of the material, the main reason is that the axial thermal expansion coefficient of the carbon fiber is equivalent to that of the micro silicon powder, meanwhile, the spiral nano-pore silicon-doped carbon fiber also has nano pores, so that the influence on the heat insulation performance is small, and meanwhile, due to the existence of the three-dimensional structure of the spiral structure, the distribution is more uniform in the raw material mixing process, so that the stability and the heat insulation performance of the material are better.
As can be seen from table 3, the addition of the reinforced fiber membrane and the helical nanoporous silicon-doped carbon fiber is beneficial to the increase of the mechanical properties of the material, and the main reason is that the reinforced fiber membrane is of a three-dimensional structure and can effectively transfer load from the matrix to the reinforcement, thereby improving the bonding strength and the mechanical properties. The three-dimensional structure of the spiral nanopore silicon-doped carbon fiber not only plays a role in uniformly dispersing raw materials in raw material mixing and preventing agglomeration, but also has a special three-dimensional structure, the fracture behavior shows typical step fracture of the three-dimensional structure, and the fracture toughness is greatly improved compared with that of a two-dimensional structure, which can be seen from the data of example 5 and comparative example 3.

Claims (10)

1. A nanometer heat insulating material is characterized in that: comprises the following components in percentage by weight: 3-9% of a reinforced fiber membrane, 5-10% of nano-pore silicon-doped carbon fiber, 5-10% of an opacifier and the balance of modified silica fume with the particle size of 10-100 nm; wherein the content of the first and second substances,
the structure of the nano-pore silicon-doped carbon fiber is a spiral structure.
2. The nano-insulation material as claimed in claim 1, wherein: the diameter of the spiral structure is 0.1-0.5mm, and the height is 1-2mm.
3. The nano-insulation material according to claim 1, wherein: the pore diameter of the nanometer pore silicon-doped carbon fiber is less than or equal to 50nm.
4. The nano-insulation material according to claim 1, wherein: the reinforced fiber membrane is an ordered quartz fiber membrane, the pore diameter of pores is less than or equal to 50nm, and the diameter of quartz fibers is 400nm.
5. The nano-insulation material according to claim 4, wherein: the preparation method of the ordered quartz fiber membrane comprises the following steps:
1) Taking 100 parts of silica sol with the particle size of 5-100nm and the solid content of 20-40wt.%, and adjusting the pH value to 4;
2) Adding 100 parts of polyethylene glycol and 1 part of alumina sol, mixing and stirring uniformly, standing and defoaming to obtain a spinning solution;
3) Adding the spinning solution into an injector of an electrostatic spinning device, and applying direct current high voltage to spray the solution;
4) Receiving the ordered fiber by a rotating winding drum, wherein the voltage is 12kV, the flow is 0.5mL/h, the distance between a needle head and the winding drum is 20cm, and the rotating speed of an electric spindle is 8000r/min;
5) Drying the ordered fiber, calcining in a kiln, slowly heating to 1300 ℃ after 25 hours, and carrying out heat preservation and calcination for 8 hours;
6) Taking out and crushing to obtain ordered quartz fiber films with the length and the width of 1mm multiplied by 1mm respectively.
6. The nano-insulation material according to claim 1, wherein: the preparation method of the nano-pore silicon-doped carbon fiber comprises the following steps:
(1) Preparing polyacrylonitrile solution with the content of 6-10wt.% by adopting N', N-dimethylformamide, standing and performing vacuum defoaming to obtain spinning solution;
(2) Placing in an electrostatic spinning device, receiving by a receiving plate, and fixing a spiral calcium carbonate model on the receiving plate, wherein the spinning voltage is 14-20kV, and the spinning distance is 12-20cm;
(3) Taking down and sintering the polyacrylonitrile fiber with the nano-pore spiral structure;
(4) Washing with dilute hydrochloric acid to obtain the carbon fiber with the nano-pore spiral structure;
(5) And (3) soaking the carbon fiber with the nano-pore spiral structure in tetraethoxysilane with the concentration, taking out and drying to obtain the carbon fiber.
7. The nano-insulation material as claimed in claim 6, wherein: the sintering method comprises the following steps: pre-oxidizing at 250-260 deg.c for 1.5-2.5 hr, and carbonizing at 800-1100 deg.c for 1 hr.
8. The nano-insulation material as claimed in claim 1, wherein: the preparation method of the modified micro silicon powder comprises the following steps: dispersing the micro silicon powder in water uniformly, adding dopamine hydrochloride, adjusting the pH value to 7.5-10.5, reacting, washing and drying the product to obtain the product.
9. The nano-insulation material as claimed in claim 8, wherein: the micro silicon powder is recovered by an alloy electric furnace dust removal system, and the specific surface area is 15-27m 2 The purity is more than or equal to 99 percent per gram.
10. A preparation method of a nanometer heat insulation material is characterized by comprising the following steps: the method comprises the following steps:
(1) Taking the reinforced fiber, the modified silica fume with the particle size of 10-100nm, the opacifier and the nano-pore silicon-doped carbon fiber, placing the materials in a high-speed stirrer, and mixing the materials at the rotating speed of 500r/min for 10min;
(2) Mixing materials at a rotating speed of 1500r/min for 15min to be uniformly mixed;
(3) The sample is prepared by dry pressing under the pressure of 0.1MPa, and the sample is dried in an oven at the temperature of 110 ℃ for 12 hours.
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