CN111517748B - High-strength glass fiber composite material and preparation method thereof - Google Patents

High-strength glass fiber composite material and preparation method thereof Download PDF

Info

Publication number
CN111517748B
CN111517748B CN202010355592.4A CN202010355592A CN111517748B CN 111517748 B CN111517748 B CN 111517748B CN 202010355592 A CN202010355592 A CN 202010355592A CN 111517748 B CN111517748 B CN 111517748B
Authority
CN
China
Prior art keywords
parts
stirring
spinning
placing
oxide
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN202010355592.4A
Other languages
Chinese (zh)
Other versions
CN111517748A (en
CN111517748B8 (en
Inventor
虞晖
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Linggong Protective Equipment Hubei Co ltd
Original Assignee
Yueqing Fengjie Electronic Technology Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Yueqing Fengjie Electronic Technology Co Ltd filed Critical Yueqing Fengjie Electronic Technology Co Ltd
Priority to CN202110085841.7A priority Critical patent/CN112573893A/en
Priority to CN202110085842.1A priority patent/CN112694313A/en
Priority to CN202010355592.4A priority patent/CN111517748B8/en
Publication of CN111517748A publication Critical patent/CN111517748A/en
Publication of CN111517748B publication Critical patent/CN111517748B/en
Application granted granted Critical
Publication of CN111517748B8 publication Critical patent/CN111517748B8/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03BMANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B37/00Manufacture or treatment of flakes, fibres, or filaments from softened glass, minerals, or slags
    • C03B37/01Manufacture of glass fibres or filaments
    • C03B37/02Manufacture of glass fibres or filaments by drawing or extruding, e.g. direct drawing of molten glass from nozzles; Cooling fins therefor
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C13/00Fibre or filament compositions
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B14/00Use 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
    • C04B14/02Granular materials, e.g. microballoons
    • C04B14/022Carbon
    • C04B14/024Graphite
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B14/00Use 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
    • C04B14/38Fibrous materials; Whiskers
    • C04B14/42Glass
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B16/00Use of organic materials as fillers, e.g. pigments, for mortars, concrete or artificial stone; Treatment of organic materials specially adapted to enhance their filling properties in mortars, concrete or artificial stone
    • C04B16/04Macromolecular compounds
    • C04B16/06Macromolecular compounds fibrous
    • C04B16/0675Macromolecular compounds fibrous from polymers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • C04B16/0683Polyesters, e.g. polylactides
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B24/00Use of organic materials as active ingredients for mortars, concrete or artificial stone, e.g. plasticisers
    • C04B24/24Macromolecular compounds
    • C04B24/36Bituminous materials, e.g. tar, pitch
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B28/00Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
    • C04B28/24Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing alkyl, ammonium or metal silicates; containing silica sols
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00General methods for the manufacture of artificial filaments or the like
    • D01F1/02Addition of substances to the spinning solution or to the melt
    • D01F1/10Other agents for modifying properties
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F6/00Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/88Monocomponent 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
    • D01F6/92Monocomponent 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 polyesters
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2201/00Mortars, concrete or artificial stone characterised by specific physical values
    • C04B2201/30Mortars, concrete or artificial stone characterised by specific physical values for heat transfer properties such as thermal insulation values, e.g. R-values
    • C04B2201/32Mortars, concrete or artificial stone characterised by specific physical values for heat transfer properties such as thermal insulation values, e.g. R-values for the thermal conductivity, e.g. K-factors
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2201/00Mortars, concrete or artificial stone characterised by specific physical values
    • C04B2201/50Mortars, concrete or artificial stone characterised by specific physical values for the mechanical strength

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Structural Engineering (AREA)
  • General Chemical & Material Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Textile Engineering (AREA)
  • Civil Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Glass Compositions (AREA)

Abstract

The invention discloses a high-strength glass fiber composite material and a preparation method thereof, wherein the composite material comprises the following raw materials: 10-15 parts of glass fiber, 10-15 parts of spinning fiber, 5-8 parts of additive, 20-25 parts of ethyl orthosilicate and 20-30 parts of ethanol; the glass fiber comprises the following raw materials in parts by weight: by weight, 60-65 parts of silicon dioxide, 20-25 parts of aluminum oxide, 10-15 parts of calcium oxide, 8-12 parts of magnesium oxide, 2-5 parts of zinc oxide and 1-1.5 parts of cerium dioxide. The glass fiber composite material with excellent heat-insulating property is prepared by utilizing the components such as silicon dioxide, graphene oxide and the like, has excellent mechanical property, contains the components such as spinning fiber and additives, can store heat and adjust temperature in a high-temperature environment, greatly improves the thermal stability of the composite material, can be applied to multiple fields, and has higher practicability.

Description

High-strength glass fiber composite material and preparation method thereof
Technical Field
The invention relates to the technical field of heat insulation materials, in particular to a high-strength glass fiber composite material and a preparation method thereof.
Background
Thermal insulation materials (also called thermal insulation materials) can be widely used in the industrial fields of oil exploitation, oil refining, thermal power plant pipeline thermal insulation, furnace body thermal insulation, prefabricated thermal insulation pipes and the like, the building fields of building interior walls, roofs, house floors, and the like, the field of die-casting furnaces, the thermal insulation of escape capsules, the thermal insulation of automobile engines and exhaust pipes and the like, and are widely applied.
At present, the market of the heat insulation materials mainly takes heat insulation materials such as fibers, organic foams, perlite and the like as main materials, but the heat insulation materials have poor mechanical properties and thermal stability, cannot meet the requirements of people in actual use, and bring inconvenience to people.
Aiming at the problem, a high-strength glass fiber composite material and a preparation method thereof are designed, which are one of the technical problems to be solved urgently.
Disclosure of Invention
The invention aims to provide a high-strength glass fiber composite material and a preparation method thereof, and aims to solve the problems in the prior art.
In order to achieve the purpose, the invention provides the following technical scheme:
a high-strength glass fiber composite material comprises the following raw materials in parts by weight: 10-15 parts of glass fiber, 10-15 parts of spinning fiber, 5-8 parts of additive, 20-25 parts of ethyl orthosilicate and 20-30 parts of ethanol.
According to an optimized scheme, the glass fiber comprises the following raw materials in parts by weight: by weight, 60-65 parts of silicon dioxide, 20-25 parts of aluminum oxide, 10-15 parts of calcium oxide, 8-12 parts of magnesium oxide, 2-5 parts of zinc oxide and 1-1.5 parts of cerium dioxide.
According to an optimized scheme, the spinning fiber comprises the following raw materials in parts by weight: 10-15 parts of palmitic acid, 8-12 parts of stearic acid, 5-8 parts of carbon nano tube, 10-20 parts of polyethylene glycol terephthalate, 16-25 parts of dichloromethane and 16-19 parts of trifluoroacetic acid.
According to an optimized scheme, the additive comprises the following raw materials in parts by weight: by weight, 5-8 parts of graphene oxide, 3-6 parts of a reducing agent, 20-25 parts of stearic acid, 5-9 parts of expanded graphite and 18-24 parts of paraffin.
In an optimized scheme, the reducing agent is sodium bisulfite.
According to an optimized scheme, the preparation method of the high-strength glass fiber composite material comprises the following steps:
1) preparing materials;
2) preparing glass fibers:
3) preparing spinning fibers:
4) preparation of the additive:
5) preparing silicon dioxide sol;
6) and (3) taking the silica sol, adding spinning fibers, glass fibers and additives, and preparing the composite material.
The optimized scheme comprises the following steps:
1) preparing materials;
2) preparing glass fibers: taking silicon dioxide, aluminum oxide, calcium oxide, magnesium oxide, zinc oxide and cerium dioxide, stirring and mixing, heating to 1550-;
3) preparing spinning fibers:
a) mixing palmitic acid and stearic acid under stirring, keeping the temperature in an oven at 90-100 ℃ for 2-2.5h, keeping the temperature, placing in an ultrasonic water bath, ultrasonically vibrating, and cooling at room temperature to obtain a material A;
b) placing a carbon nano tube in a pretreatment solution, stirring, carrying out ultrasonic oscillation, carrying out vacuum filtration, washing to be neutral, and then placing in a vacuum drying oven for drying to obtain a pretreated carbon nano tube;
c) dissolving polyethylene terephthalate, dichloromethane and trifluoroacetic acid mixed solution, stirring, adding the material A, stirring, adding the pretreated carbon nano tube, performing ultrasonic treatment, and continuously stirring to obtain spinning solution; taking the spinning solution, placing the spinning solution in an injector, and spinning to obtain spinning fibers;
4) preparation of the additive:
a) taking a graphene oxide solution, performing ultrasonic dispersion, adding a reducing agent and stearic acid, mixing and stirring, placing in an oven at 90-95 ℃ for reaction for 3-3.5h, washing with water, and freeze-drying to obtain modified graphene;
b) taking the expanded graphite, acidifying, heating to 800-810 ℃, and heating for expansion for 25-30s to obtain a material B; taking paraffin, heating and stirring until the paraffin is molten, adding the material B, stirring, adding the modified graphene, and continuously stirring to obtain an additive;
5) heating ethyl orthosilicate, ethanol and deionized water to 45-50 ℃, stirring, adding hydrochloric acid, adjusting the pH to 3-4, continuing stirring, slowly dropwise adding ammonia water, adjusting the pH to 7-8, and continuing stirring to obtain silicon dioxide sol;
6) adding the spinning fiber and the glass fiber into the silica sol, stirring, adding the additive, continuously stirring, aging, cleaning with ethanol, aging in ethanol, cleaning with n-hexane, continuously aging in n-hexane, and drying to obtain the composite material.
The optimized scheme comprises the following steps:
1) preparing materials;
2) preparing glass fibers: taking silicon dioxide, aluminum oxide, calcium oxide, magnesium oxide, zinc oxide and cerium dioxide, stirring and mixing for 30-40min, heating to 1550-; the preparation of the glass fiber is carried out in the step 2), wherein the glass fiber comprises components such as silicon dioxide, aluminum oxide, calcium oxide, magnesium oxide, zinc oxide, cerium dioxide and the like, and the silicon dioxide is a main network former of the glass fiber and can be used as a framework structure of the glass fiber; the addition of the aluminum oxide can improve the chemical stability of the glass fiber, and the aluminum oxide tetrahedron coordination structure participates in the network structure of the glass fiber to improve the melting property and the devitrification property of the glass fiber; the calcium oxide and the magnesium oxide can provide exo ions of a network structure, so that the glass network structure is more compact, and the chemical stability and the mechanical property of the glass fiber are improved; the cerium dioxide is used as a rich rare earth resource, the addition cost is low, the high-temperature viscosity of the glass can be reduced, the valence change reaction is carried out at high temperature to generate oxygen, the clarification effect can be achieved in the preparation process of the glass fiber, the connection of a glass network framework is promoted, the bridge oxygen in the glass network structure is increased, the structure of the glass fiber is more compact, and the mechanical property and the chemical stability are improved.
3) Preparing spinning fibers:
a) mixing palmitic acid and stearic acid under stirring for 20-30min, keeping the temperature in an oven at 90-100 deg.C for 2-2.5h, placing in an ultrasonic water bath at 80-82 deg.C, ultrasonically vibrating for 2-3min, and cooling at room temperature to obtain material A;
b) placing the carbon nano tube in a pretreatment solution, stirring for 20-30min, ultrasonically oscillating for 5-5.5h, vacuum filtering, washing to be neutral, and then placing in a vacuum drying oven at 90-100 ℃ for drying to obtain a pretreated carbon nano tube;
c) dissolving polyethylene terephthalate, dichloromethane and trifluoroacetic acid mixed solution, stirring for 15-20min, adding material A, stirring for 20-30min, adding pretreated carbon nanotube, performing ultrasonic treatment for 3-5min, and continuously stirring for 25-30min to obtain spinning solution; taking the spinning solution, placing the spinning solution in an injector, and spinning to obtain spinning fibers; the preparation of the spinning fiber is carried out in the step 3) of the application, the spinning fiber comprises palmitic acid, stearic acid, carbon nano tubes and other components, a large amount of carboxyl and hydroxyl are distributed on the surface of the acidified nano tubes, the acidified nano tubes can be combined with carbonyl of polyethylene glycol terephthalate and carboxyl in dibasic fatty acid in a reaction mode, rich grooves are distributed on the surface of the obtained spinning fiber, a solid-liquid phase change material is prepared by adopting a method combining melt mixing and ultrasonic oscillation during preparation, the spinning fiber is prepared by utilizing an electrostatic spinning method, the spinning fiber has excellent heat storage and temperature regulation performance, heat storage and temperature regulation can be carried out on heat conducted in the composite material, and the heat stability of the composite material is greatly improved.
4) Preparation of the additive:
a) taking a graphene oxide solution, carrying out ultrasonic dispersion for 10-15min, adding a reducing agent and stearic acid, mixing and stirring for 10-15min, placing in an oven at 90-95 ℃ for reaction for 3-3.5h, washing with water, and carrying out freeze drying to obtain modified graphene;
b) taking the expanded graphite, acidifying, heating to 800-810 ℃, and heating for expansion for 25-30s to obtain a material B; heating paraffin to 80-90 ℃, stirring until the paraffin is molten, adding the material B, stirring for 1-1.2h, adding the modified graphene, and continuously stirring for 10-20min to obtain an additive; the additive prepared in the step 4) of the application comprises components such as graphene oxide, expanded graphite, paraffin and the like, wherein the graphene oxide can be used for preparing graphene aerogel, and the graphene aerogel is a carbon material with a porous net structure and can adsorb and coat the phase-change material, so that the heat transfer rate of the phase-change material is improved; the expanded graphite is a loose and porous vermicular substance obtained by intercalating, washing, drying and high-temperature expanding natural crystalline flake graphite, and has a large amount of network microporous structures, large specific surface area and high surface activity, so that the expanded graphite has good adsorption and coating properties; therefore, the graphene aerogel is matched with the expanded graphite to coat the paraffin, the additive is prepared, the additive has an excellent heat storage and temperature regulation effect, the additive and the spinning fiber are added into the silica sol together, and the prepared composite material has excellent thermal stability.
5) Heating ethyl orthosilicate, ethanol and deionized water to 45-50 ℃, stirring for 10-20min, adding hydrochloric acid, adjusting the pH to 3-4, continuing to stir for 2-2.5h, slowly dropwise adding ammonia water, adjusting the pH to 7-8, and continuing to stir for 10-15min to obtain silicon dioxide sol; preparing silicon dioxide sol in step 5);
6) adding the spinning fiber and the glass fiber into the silica sol, stirring for 20-30min, adding the additive, continuously stirring for 20-30min, aging for 24-26h, cleaning with ethanol, aging in ethanol for 24-26h, cleaning with n-hexane, continuously aging in n-hexane for 8-9h, and drying at 80-90 ℃ for 6-8h to obtain the composite material. In the step 6), the spinning fiber and the glass fiber are added into the silica sol, the spinning fiber and the glass fiber not only can play a role in supporting a framework and transferring stress, and the mechanical property of the composite material can be improved, but also the spinning fiber and the additive are matched with each other, so that the composite material has a relatively excellent heat storage and temperature regulation effect, the thermal stability of the composite material can be greatly improved, meanwhile, the composite material selects silica aerogel as a main body structure, the graphene oxide and the glass fiber both have certain heat insulation performance, and the prepared composite material is low in heat conductivity coefficient and excellent in heat insulation performance.
In the optimized scheme, in the step 2), the drawing temperature is 1340-1350 ℃, the drawing speed is 500-1250r/min, and the drawing time is 30-35 s.
According to an optimized scheme, in the step b) of the step 3), the pretreatment solution is a mixed solution of nitric acid and sulfuric acid, and the volume ratio of the nitric acid to the sulfuric acid is 1: (2-3).
Compared with the prior art, the invention has the beneficial effects that:
the invention discloses a high-strength glass fiber composite material and a preparation method thereof, the process design is reasonable, the component proportion is simple, the glass fiber composite material with excellent heat insulation performance is prepared by utilizing components such as silicon dioxide, graphene oxide and the like, the composite material has excellent mechanical property, and meanwhile, the composite material contains components such as spinning fibers, additives and the like, so that the heat storage and temperature adjustment can be carried out on the composite material in a high-temperature environment, the thermal stability of the composite material is greatly improved, the composite material can be applied to multiple fields, and the high-strength glass fiber composite material has high practicability.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
s1: preparing materials;
s2: preparing glass fibers:
taking silicon dioxide, aluminum oxide, calcium oxide, magnesium oxide, zinc oxide and cerium dioxide, stirring and mixing for 30min, heating to 1550 ℃, carrying out heat preservation reaction for 10h, then placing glass liquid in a mold for processing and molding, annealing after molding, keeping the temperature for 1h at the annealing temperature of 600 ℃, cooling along with a furnace, placing in a wire drawing machine for wire drawing after cooling, wherein the wire drawing temperature is 1340 ℃, the wire drawing speed is 500r/min, and the wire drawing time is 30s, thus obtaining the glass fiber;
s3: preparing spinning fibers:
mixing palmitic acid and stearic acid under stirring for 20min, keeping the temperature in an oven at 90 ℃ for 2h, placing in an ultrasonic water bath at 80 ℃, ultrasonically vibrating for 2min, and cooling at room temperature to obtain a material A;
placing a carbon nano tube in the pretreatment solution, stirring for 20min, ultrasonically oscillating for 5h, carrying out vacuum filtration, washing to be neutral, and then placing in a vacuum drying oven at 90 ℃ for drying to obtain a pretreated carbon nano tube; the pretreatment solution is a mixed solution of nitric acid and sulfuric acid, and the volume ratio of the nitric acid to the sulfuric acid is 1: 2;
dissolving polyethylene terephthalate, dichloromethane and trifluoroacetic acid mixed solution, stirring for 15min, adding the material A, stirring for 20min, adding the pretreated carbon nanotube, performing ultrasonic treatment for 3min, and continuously stirring for 25min to obtain spinning solution; taking the spinning solution, placing the spinning solution in an injector, and spinning to obtain spinning fibers;
s4: preparation of the additive:
taking a graphene oxide solution, carrying out ultrasonic dispersion for 10min, adding a reducing agent and stearic acid, mixing and stirring for 10min, placing in a 90 ℃ oven for reaction for 3h, washing with water, and freeze-drying to obtain modified graphene;
taking expanded graphite, acidifying, heating to 800 ℃, and expanding for 25s to obtain a material B; taking paraffin, heating to 80 ℃, stirring until the paraffin is molten, adding the material B, stirring for 1h, adding the modified graphene, and continuously stirring for 10min to obtain an additive;
s5: preparation of silica sol:
heating ethyl orthosilicate, ethanol and deionized water to 45 ℃, stirring for 10min, adding hydrochloric acid, adjusting the pH to 3, continuing stirring for 2h, slowly dropwise adding ammonia water, adjusting the pH to 7, and continuing stirring for 10min to obtain silicon dioxide sol;
s6: adding the spinning fiber and the glass fiber into the silica sol, stirring for 20min, adding the additive, continuously stirring for 20min, aging for 24h, cleaning with ethanol, aging in ethanol for 24h, cleaning with n-hexane, continuously aging in n-hexane for 8h, and drying at 80 ℃ for 6h to obtain the composite material.
In this embodiment, the composite material comprises the following raw materials: 10 parts of glass fiber, 10 parts of spinning fiber, 5 parts of additive, 20 parts of ethyl orthosilicate and 20 parts of ethanol.
Wherein the glass fiber comprises the following raw materials in parts by weight: by weight, 60 parts of silicon dioxide, 20 parts of aluminum oxide, 10 parts of calcium oxide, 8 parts of magnesium oxide, 2 parts of zinc oxide and 1 part of cerium dioxide. The spinning fiber comprises the following raw materials in parts by weight: 10 parts of palmitic acid, 8 parts of stearic acid, 5 parts of carbon nano tube, 10 parts of polyethylene terephthalate, 16 parts of dichloromethane and 16 parts of trifluoroacetic acid.
The additive comprises the following raw materials: by weight, 5 parts of graphene oxide, 3 parts of a reducing agent, 20 parts of stearic acid, 5 parts of expanded graphite and 18 parts of paraffin. The reducing agent is sodium bisulfite.
Example 2:
s1: preparing materials;
s2: preparing glass fibers:
taking silicon dioxide, aluminum oxide, calcium oxide, magnesium oxide, zinc oxide and cerium dioxide, stirring and mixing for 35min, heating to 1555 ℃, carrying out heat preservation reaction for 11h, then placing glass liquid in a mold for processing and molding, annealing after molding, keeping the annealing temperature at 605 ℃, carrying out heat preservation for 1.2h, cooling along with a furnace, placing in a wire drawing machine for wire drawing after cooling, wherein the wire drawing temperature is 1345 ℃, the wire drawing speed is 1000r/min, and the wire drawing time is 33s, so as to obtain glass fibers;
s3: preparing spinning fibers:
mixing palmitic acid and stearic acid under stirring for 25min, keeping the temperature in an oven at 95 ℃ for 2.3h, placing in an ultrasonic water bath at 81 ℃, ultrasonically vibrating for 2.5min, and cooling at room temperature to obtain a material A;
placing a carbon nano tube in the pretreatment solution, stirring for 25min, ultrasonically oscillating for 5.2h, carrying out vacuum filtration, washing to be neutral, and then placing in a vacuum drying oven at 95 ℃ for drying to obtain a pretreated carbon nano tube; the pretreatment solution is a mixed solution of nitric acid and sulfuric acid, and the volume ratio of the nitric acid to the sulfuric acid is 1: 2.5;
dissolving polyethylene terephthalate, dichloromethane and trifluoroacetic acid mixed solution, stirring for 18min, adding the material A, stirring for 25min, adding the pretreated carbon nanotube, performing ultrasonic treatment for 4min, and continuously stirring for 28min to obtain spinning solution; taking the spinning solution, placing the spinning solution in an injector, and spinning to obtain spinning fibers;
s4: preparation of the additive:
taking a graphene oxide solution, carrying out ultrasonic dispersion for 13min, adding a reducing agent and stearic acid, mixing and stirring for 12min, placing in a 92 ℃ oven for reaction for 3.2h, washing with water, and freeze-drying to obtain modified graphene;
taking expanded graphite, acidifying, heating to 805 ℃, and heating for expansion for 28s to obtain a material B; taking paraffin, heating to 85 ℃, stirring until the paraffin is molten, adding the material B, stirring for 1.1h, adding the modified graphene, and continuously stirring for 15min to obtain an additive;
s5: preparation of silica sol:
heating ethyl orthosilicate, ethanol and deionized water to 48 ℃, stirring for 18min, adding hydrochloric acid, adjusting the pH to 3.5, continuing to stir for 2.2h, slowly dropwise adding ammonia water, adjusting the pH to 7.5, and continuing to stir for 12min to obtain silicon dioxide sol;
s6: adding the spinning fiber and the glass fiber into the silica sol, stirring for 25min, adding the additive, continuously stirring for 28min, aging for 25h, cleaning with ethanol, aging in ethanol for 25h, cleaning with n-hexane, continuously aging in n-hexane for 8.5h, and drying at 85 ℃ for 7h to obtain the composite material.
In this embodiment, the composite material comprises the following raw materials: by weight, 12 parts of glass fiber, 13 parts of spinning fiber, 7 parts of additive, 22 parts of ethyl orthosilicate and 25 parts of ethanol.
Wherein the glass fiber comprises the following raw materials in parts by weight: by weight, 61 parts of silicon dioxide, 24 parts of aluminum oxide, 12 parts of calcium oxide, 10 parts of magnesium oxide, 4 parts of zinc oxide and 1.2 parts of cerium dioxide. The spinning fiber comprises the following raw materials in parts by weight: by weight, 14 parts of palmitic acid, 10 parts of stearic acid, 6 parts of carbon nano tube, 18 parts of polyethylene terephthalate, 21 parts of dichloromethane and 18 parts of trifluoroacetic acid.
The additive comprises the following raw materials: by weight, 7 parts of graphene oxide, 5 parts of a reducing agent, 24 parts of stearic acid, 8 parts of expanded graphite and 22 parts of paraffin. The reducing agent is sodium bisulfite.
Example 3:
s1: preparing materials;
s2: preparing glass fibers:
taking silicon dioxide, aluminum oxide, calcium oxide, magnesium oxide, zinc oxide and cerium dioxide, stirring and mixing for 40min, heating to 1560 ℃, carrying out heat preservation reaction for 12h, then placing glass liquid in a mold for processing and molding, annealing after molding, keeping the temperature for 1.5h at the annealing temperature of 610 ℃, cooling along with a furnace, placing in a wire drawing machine for wire drawing after cooling, wherein the wire drawing temperature is 1350 ℃, the wire drawing speed is 1250r/min, and the wire drawing time is 35s, thus obtaining the glass fiber;
s3: preparing spinning fibers:
mixing palmitic acid and stearic acid under stirring for 30min, keeping the temperature in an oven at 100 ℃ for 2.5h, placing in an ultrasonic water bath at 82 ℃ after keeping the temperature, ultrasonically vibrating for 3min, and cooling at room temperature to obtain a material A;
placing a carbon nano tube in the pretreatment solution, stirring for 30min, ultrasonically oscillating for 5.5h, carrying out vacuum filtration, washing to be neutral, and then placing in a vacuum drying oven at 100 ℃ for drying to obtain a pretreated carbon nano tube; the pretreatment solution is a mixed solution of nitric acid and sulfuric acid, and the volume ratio of the nitric acid to the sulfuric acid is 1: 3;
dissolving polyethylene terephthalate, dichloromethane and trifluoroacetic acid mixed solution, stirring for 20min, adding the material A, stirring for 30min, adding the pretreated carbon nanotube, performing ultrasonic treatment for 5min, and continuously stirring for 30min to obtain spinning solution; taking the spinning solution, placing the spinning solution in an injector, and spinning to obtain spinning fibers;
s4: preparation of the additive:
taking a graphene oxide solution, carrying out ultrasonic dispersion for 15min, adding a reducing agent and stearic acid, mixing and stirring for 15min, placing in a 95 ℃ oven for reaction for 3.5h, washing with water, and freeze-drying to obtain modified graphene;
taking expanded graphite, acidifying, heating to 810 ℃, and heating for expansion for 30s to obtain a material B; taking paraffin, heating to 90 ℃, stirring until the paraffin is molten, adding the material B, stirring for 1.2h, adding the modified graphene, and continuously stirring for 20min to obtain an additive;
s5: preparation of silica sol:
heating ethyl orthosilicate, ethanol and deionized water to 50 ℃, stirring for 20min, adding hydrochloric acid, adjusting the pH to 4, continuing to stir for 2.5h, slowly dropwise adding ammonia water, adjusting the pH to 8, and continuing to stir for 15min to obtain silicon dioxide sol;
s6: adding the spinning fiber and the glass fiber into the silica sol, stirring for 30min, adding the additive, continuously stirring for 30min, aging for 26h, cleaning with ethanol, aging in ethanol for 26h, cleaning with n-hexane, continuously aging in n-hexane for 9h, and drying at 90 ℃ for 8h to obtain the composite material.
In this embodiment, the composite material comprises the following raw materials: by weight, 15 parts of glass fiber, 15 parts of spinning fiber, 8 parts of additive, 25 parts of ethyl orthosilicate and 30 parts of ethanol.
Wherein the glass fiber comprises the following raw materials in parts by weight: by weight, 65 parts of silicon dioxide, 25 parts of aluminum oxide, 15 parts of calcium oxide, 12 parts of magnesium oxide, 5 parts of zinc oxide and 1.5 parts of cerium dioxide. The spinning fiber comprises the following raw materials in parts by weight: by weight, 15 parts of palmitic acid, 12 parts of stearic acid, 8 parts of carbon nano tube, 20 parts of polyethylene terephthalate, 25 parts of dichloromethane and 19 parts of trifluoroacetic acid.
The additive comprises the following raw materials: by weight, 8 parts of graphene oxide, 6 parts of a reducing agent, 25 parts of stearic acid, 9 parts of expanded graphite and 24 parts of paraffin. The reducing agent is sodium bisulfite.
Experiment 1:
1. taking the composite materials prepared in the examples 1-3, respectively adopting an HFM436/3/0 heat conductivity coefficient tester to test the heat conductivity coefficient of the materials according to GB/T10295-2008 ' determination of steady-state thermal resistance and related characteristics of heat-insulating materials ' heat flow meter method ';
2. the composite materials prepared in examples 1 to 3 were tested for their compression properties by means of a universal tester (sample size 30 mm. times.30 mm. times.6 mm, loading rate 2 mm/min).
Specific data can be shown in the following table:
item Example 1 Example 2 Example 3
Compressive Strength (30% pressure Change)/KPa 24.68 25.13 25.11
Compressive Strength (60% pressure Change)/KPa 190.25 193.51 192.47
Coefficient of thermal conductivity (W.m)-1·K-1) 0.023 0.021 0.024
3. The composite materials prepared in examples 1-3 were tested for thermal stability in air atmosphere (air flow rate 50mL/min, temperature range 40-1000 deg.C, temperature rise rate 20 deg.C/min) using SDTQ600 thermogravimetry-differential thermal analyzer (TG-DTA)
After experiments, the composite material prepared by the invention has excellent thermal stability, the total mass loss of the composite material is 3.2-3.4% when the experiment temperature is increased to 650 ℃, and the total mass loss of the composite material is 3.9-4.1% when the experiment temperature is increased to 1000 ℃.
And (4) conclusion: according to the invention, the glass fiber composite material with excellent heat-insulating property is prepared by utilizing components such as silicon dioxide and graphene oxide, the composite material has excellent mechanical property, and meanwhile, the glass fiber composite material contains components such as spinning fiber and additives, so that the composite material can be subjected to heat storage and temperature adjustment in a high-temperature environment, the thermal stability of the composite material is greatly improved, and the glass fiber composite material can be applied to multiple fields and has higher practicability.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.

Claims (5)

1. A high-strength glass fiber composite material is characterized in that: the composite material comprises the following raw materials in parts by weight: 10-15 parts of glass fiber, 10-15 parts of spinning fiber, 5-8 parts of additive, 20-25 parts of ethyl orthosilicate and 20-30 parts of ethanol;
the glass fiber comprises the following raw materials in parts by weight: 60-65 parts of silicon dioxide, 20-25 parts of aluminum oxide, 10-15 parts of calcium oxide, 8-12 parts of magnesium oxide, 2-5 parts of zinc oxide and 1-1.5 parts of cerium dioxide by weight;
the spinning fiber comprises the following raw materials in parts by weight: 10-15 parts of palmitic acid, 8-12 parts of stearic acid, 5-8 parts of carbon nano tube, 10-20 parts of polyethylene glycol terephthalate, 16-25 parts of dichloromethane and 16-19 parts of trifluoroacetic acid;
the additive comprises the following raw materials in parts by weight: 5-8 parts of graphene oxide, 3-6 parts of a reducing agent, 20-25 parts of stearic acid, 5-9 parts of expanded graphite and 18-24 parts of paraffin by weight;
the preparation method comprises the following steps:
1) preparing materials;
2) preparing glass fibers: taking silicon dioxide, aluminum oxide, calcium oxide, magnesium oxide, zinc oxide and cerium dioxide, stirring and mixing, heating to 1550-;
3) preparing spinning fibers:
a) mixing palmitic acid and stearic acid under stirring, keeping the temperature in an oven at 90-100 ℃ for 2-2.5h, keeping the temperature, placing in an ultrasonic water bath, ultrasonically vibrating, and cooling at room temperature to obtain a material A;
b) placing a carbon nano tube in a pretreatment solution, stirring, carrying out ultrasonic oscillation, carrying out vacuum filtration, washing to be neutral, and then placing in a vacuum drying oven for drying to obtain a pretreated carbon nano tube;
c) dissolving polyethylene terephthalate, dichloromethane and trifluoroacetic acid mixed solution, stirring, adding the material A, stirring, adding the pretreated carbon nano tube, performing ultrasonic treatment, and continuously stirring to obtain spinning solution; taking the spinning solution, placing the spinning solution in an injector, and spinning to obtain spinning fibers;
4) preparation of the additive:
a) taking a graphene oxide solution, performing ultrasonic dispersion, adding a reducing agent and stearic acid, mixing and stirring, placing in an oven at 90-95 ℃ for reaction for 3-3.5h, washing with water, and freeze-drying to obtain modified graphene;
b) taking the expanded graphite, acidifying, heating to 800-810 ℃, and heating for expansion for 25-30s to obtain a material B; taking paraffin, heating and stirring until the paraffin is molten, adding the material B, stirring, adding the modified graphene, and continuously stirring to obtain an additive;
5) heating ethyl orthosilicate, ethanol and deionized water to 45-50 ℃, stirring, adding hydrochloric acid, adjusting the pH to 3-4, continuing stirring, slowly dropwise adding ammonia water, adjusting the pH to 7-8, and continuing stirring to obtain silicon dioxide sol;
6) adding the spinning fiber and the glass fiber into the silica sol, stirring, adding the additive, continuously stirring, aging, cleaning with ethanol, aging in ethanol, cleaning with n-hexane, continuously aging in n-hexane, and drying to obtain the composite material.
2. A high strength fiberglass composite according to claim 1, wherein: the reducing agent is sodium bisulfite.
3. A high strength fiberglass composite according to claim 1, wherein: the method comprises the following steps:
1) preparing materials;
2) preparing glass fibers: taking silicon dioxide, aluminum oxide, calcium oxide, magnesium oxide, zinc oxide and cerium dioxide, stirring and mixing for 30-40min, heating to 1550-;
3) preparing spinning fibers:
d) mixing palmitic acid and stearic acid under stirring for 20-30min, keeping the temperature in an oven at 90-100 deg.C for 2-2.5h, placing in an ultrasonic water bath at 80-82 deg.C, ultrasonically vibrating for 2-3min, and cooling at room temperature to obtain material A;
e) placing the carbon nano tube in a pretreatment solution, stirring for 20-30min, ultrasonically oscillating for 5-5.5h, vacuum filtering, washing to be neutral, and then placing in a vacuum drying oven at 90-100 ℃ for drying to obtain a pretreated carbon nano tube;
f) dissolving polyethylene terephthalate, dichloromethane and trifluoroacetic acid mixed solution, stirring for 15-20min, adding material A, stirring for 20-30min, adding pretreated carbon nanotube, performing ultrasonic treatment for 3-5min, and continuously stirring for 25-30min to obtain spinning solution; taking the spinning solution, placing the spinning solution in an injector, and spinning to obtain spinning fibers;
4) preparation of the additive:
c) taking a graphene oxide solution, carrying out ultrasonic dispersion for 10-15min, adding a reducing agent and stearic acid, mixing and stirring for 10-15min, placing in an oven at 90-95 ℃ for reaction for 3-3.5h, washing with water, and carrying out freeze drying to obtain modified graphene;
d) taking the expanded graphite, acidifying, heating to 800-810 ℃, and heating for expansion for 25-30s to obtain a material B; heating paraffin to 80-90 ℃, stirring until the paraffin is molten, adding the material B, stirring for 1-1.2h, adding the modified graphene, and continuously stirring for 10-20min to obtain an additive;
5) heating ethyl orthosilicate, ethanol and deionized water to 45-50 ℃, stirring for 10-20min, adding hydrochloric acid, adjusting the pH to 3-4, continuing to stir for 2-2.5h, slowly dropwise adding ammonia water, adjusting the pH to 7-8, and continuing to stir for 10-15min to obtain silicon dioxide sol;
6) adding the spinning fiber and the glass fiber into the silica sol, stirring for 20-30min, adding the additive, continuously stirring for 20-30min, aging for 24-26h, cleaning with ethanol, aging in ethanol for 24-26h, cleaning with n-hexane, continuously aging in n-hexane for 8-9h, and drying at 80-90 ℃ for 6-8h to obtain the composite material.
4. A high strength fiberglass composite according to claim 3, wherein: in the step 2), the drawing temperature is 1340-1350 ℃, the drawing speed is 500-1250r/min, and the drawing time is 30-35 s.
5. A high strength fiberglass composite according to claim 3, wherein: in the step b) of the step 3), the pretreatment solution is a mixed solution of nitric acid and sulfuric acid, and the volume ratio of the nitric acid to the sulfuric acid is 1: (2-3).
CN202010355592.4A 2020-04-29 2020-04-29 High-strength glass fiber composite material and preparation method thereof Active CN111517748B8 (en)

Priority Applications (3)

Application Number Priority Date Filing Date Title
CN202110085841.7A CN112573893A (en) 2020-04-29 2020-04-29 High-strength glass fiber composite material
CN202110085842.1A CN112694313A (en) 2020-04-29 2020-04-29 High-strength glass fiber composite material
CN202010355592.4A CN111517748B8 (en) 2020-04-29 2020-04-29 High-strength glass fiber composite material and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202010355592.4A CN111517748B8 (en) 2020-04-29 2020-04-29 High-strength glass fiber composite material and preparation method thereof

Related Child Applications (2)

Application Number Title Priority Date Filing Date
CN202110085841.7A Division CN112573893A (en) 2020-04-29 2020-04-29 High-strength glass fiber composite material
CN202110085842.1A Division CN112694313A (en) 2020-04-29 2020-04-29 High-strength glass fiber composite material

Publications (3)

Publication Number Publication Date
CN111517748A CN111517748A (en) 2020-08-11
CN111517748B true CN111517748B (en) 2021-03-12
CN111517748B8 CN111517748B8 (en) 2021-03-30

Family

ID=71904736

Family Applications (3)

Application Number Title Priority Date Filing Date
CN202110085841.7A Pending CN112573893A (en) 2020-04-29 2020-04-29 High-strength glass fiber composite material
CN202010355592.4A Active CN111517748B8 (en) 2020-04-29 2020-04-29 High-strength glass fiber composite material and preparation method thereof
CN202110085842.1A Withdrawn CN112694313A (en) 2020-04-29 2020-04-29 High-strength glass fiber composite material

Family Applications Before (1)

Application Number Title Priority Date Filing Date
CN202110085841.7A Pending CN112573893A (en) 2020-04-29 2020-04-29 High-strength glass fiber composite material

Family Applications After (1)

Application Number Title Priority Date Filing Date
CN202110085842.1A Withdrawn CN112694313A (en) 2020-04-29 2020-04-29 High-strength glass fiber composite material

Country Status (1)

Country Link
CN (3) CN112573893A (en)

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114011158A (en) * 2021-11-25 2022-02-08 镇江瑞昊工程塑料有限公司 Method for modifying composite filter material by PTFE emulsion

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH01103923A (en) * 1987-10-16 1989-04-21 Asahi Glass Co Ltd Spinning solution suitable for producing silica fiber
CN1070019A (en) * 1992-09-22 1993-03-17 赖明三 A kind of processing method of antistatic antibiotic fiber
CN107012535A (en) * 2016-01-28 2017-08-04 海南大学 A kind of method for preparing graphene/glass composite fibre
CN107557913A (en) * 2017-08-01 2018-01-09 东华大学 A kind of two-dimension netted superfine carbon nano-fiber materials and preparation method thereof
CN108689624A (en) * 2018-07-06 2018-10-23 佛山陵朝新材料有限公司 A kind of high mating type discards the preparation method of rubber powder composite mortar material
CN110723905A (en) * 2019-11-05 2020-01-24 江苏华鸥玻璃有限公司 Brown high-strength reagent bottle glass material and preparation method thereof

Family Cites Families (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101973752B (en) * 2010-10-21 2013-01-23 厦门大学 Glass fiber reinforced silicon dioxide aerogel composite material and preparation method thereof
CN102557577B (en) * 2011-11-01 2014-03-19 厦门纳美特新材料科技有限公司 Preparation method of silicon dioxide aerogel composite material
CN107304052A (en) * 2016-04-22 2017-10-31 北京化工大学 A kind of preparation method of graphene oxide doped aerosil
CN107235744B (en) * 2017-06-02 2020-06-02 东南大学 Preparation method of graphene-silicon dioxide aerogel
CN107840580A (en) * 2017-12-05 2018-03-27 徐州金港起重机制造有限公司 A kind of corrosion-resistant fiberglass formula
CN108467276A (en) * 2018-03-20 2018-08-31 中国科学院城市环境研究所 A kind of preparation method of electrostatic spinning nano fiber enhancing aerosil

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH01103923A (en) * 1987-10-16 1989-04-21 Asahi Glass Co Ltd Spinning solution suitable for producing silica fiber
CN1070019A (en) * 1992-09-22 1993-03-17 赖明三 A kind of processing method of antistatic antibiotic fiber
CN107012535A (en) * 2016-01-28 2017-08-04 海南大学 A kind of method for preparing graphene/glass composite fibre
CN107557913A (en) * 2017-08-01 2018-01-09 东华大学 A kind of two-dimension netted superfine carbon nano-fiber materials and preparation method thereof
CN108689624A (en) * 2018-07-06 2018-10-23 佛山陵朝新材料有限公司 A kind of high mating type discards the preparation method of rubber powder composite mortar material
CN110723905A (en) * 2019-11-05 2020-01-24 江苏华鸥玻璃有限公司 Brown high-strength reagent bottle glass material and preparation method thereof

Also Published As

Publication number Publication date
CN111517748A (en) 2020-08-11
CN112573893A (en) 2021-03-30
CN112694313A (en) 2021-04-23
CN111517748B8 (en) 2021-03-30

Similar Documents

Publication Publication Date Title
CN105199472B (en) A kind of preparation method of airsetting matrix insulation phase-change coating
CN110804420B (en) Phase-change composite material based on high-thermal-conductivity anisotropic graphene framework and preparation method thereof
CN101219873B (en) Nano-porous thermal insulating material and method for producing the same
Jin et al. Preparation and characterization of capric-stearic acid/montmorillonite/graphene composite phase change material for thermal energy storage in buildings
CN113416028B (en) Production process of waterproof aerogel thermal insulation material
CN111517748B (en) High-strength glass fiber composite material and preparation method thereof
CN109225079A (en) A kind of high temperature resistant aeroge composite material and preparation method
CN114656262B (en) High-entropy ceramic aerogel powder with low thermal conductivity and preparation method thereof
CN115583829B (en) Low-thermal-conductivity fiber composite aerogel wet felt and preparation method thereof
CN112709075A (en) High-strength aerogel modified heat insulation felt and preparation method thereof
CN110330014B (en) Preparation method of starch porous carbon microspheres for supercapacitor electrode material
Peng et al. High-efficiency energy-saving buildings utilizing potassium tungsten bronze heat-insulating glass and polyethylene glycol/expanded energy storage blanket
CN105968789B (en) A kind of lightweight Organic-inorganic composite insulating foam and preparation method
CN108484097B (en) Preparation method of lignin-enhanced silicon dioxide aerogel felt
CN114014631A (en) Closed-cell perlite composite thermal insulation material and preparation method thereof
CN106185931A (en) A kind of preparation method of active carbon with high specific surface area
CN107935553A (en) A kind of preparation method of fire resistant environment-friendly pipe insulation material
CN115537026B (en) Polyimide aerogel and preparation method thereof
CN115975251A (en) Preparation method of heat-preservation and heat-insulation cellulose aerogel composite material
CN113736431B (en) Modified expanded graphite-hydrated inorganic salt composite phase-change material and preparation method and application thereof
CN109320882A (en) Silica modified PVDF aeroge, preparation method and the aerogel product including it
CN108675331B (en) Al (aluminum)2O3Preparation method of aerogel/carbon foam composite heat-insulating material
CN105694729A (en) Composite heat insulation coating and preparation process thereof
CN115477318B (en) Method for preparing complete block-shaped pure alumina aerogel by freeze drying
CN114836094B (en) Antistatic color-coated sheet

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
TA01 Transfer of patent application right
TA01 Transfer of patent application right

Effective date of registration: 20210225

Address after: No.152, Sanchi Road, xirendang village, Liushi Town, Yueqing City, Wenzhou City, Zhejiang Province

Applicant after: YUEQING FENGJIE ELECTRONIC TECHNOLOGY Co.,Ltd.

Address before: 215300 No.51, shaodiangang Road, Jinxi Town, Kunshan City, Suzhou City, Jiangsu Province

Applicant before: Yu Hui

GR01 Patent grant
GR01 Patent grant
TA01 Transfer of patent application right
TA01 Transfer of patent application right

Effective date of registration: 20210303

Address after: 325600 No. 493, Xinfang village, Dajing Town, Yueqing City, Wenzhou City, Zhejiang Province

Applicant after: Xu Qianqian

Address before: No.152, Sanchi Road, xirendang village, Liushi Town, Yueqing City, Wenzhou City, Zhejiang Province

Applicant before: YUEQING FENGJIE ELECTRONIC TECHNOLOGY Co.,Ltd.

CI03 Correction of invention patent
CI03 Correction of invention patent

Correction item: Patentee|Address

Correct: Xu Qianqian|325600 No.493 Xinfang Village, Dajing Town, Yueqing City, Wenzhou City, Zhejiang Province

False: Yueqing Fengjie Electronic Technology Co.,Ltd.|325600 No.152 Sanchi Road, Xirendang Village, Liushi Town, Yueqing City, Zhejiang Province

Number: 11-02

Page: The title page

Volume: 37

Correction item: Patentee|Address

Correct: Xu Qianqian|325600 No.493 Xinfang Village, Dajing Town, Yueqing City, Wenzhou City, Zhejiang Province

False: Yueqing Fengjie Electronic Technology Co.,Ltd.|325600 No.152 Sanchi Road, Xirendang Village, Liushi Town, Yueqing City, Zhejiang Province

Number: 11-02

Volume: 37

TR01 Transfer of patent right
TR01 Transfer of patent right

Effective date of registration: 20230608

Address after: 448000 East Section of Xinyang Avenue (Quchang Village), Jingshan Economic Development Zone, Jingmen City, Hubei Province

Patentee after: Linggong protective equipment (Hubei) Co.,Ltd.

Address before: 325600 No. 493, Xinfang village, Dajing Town, Yueqing City, Wenzhou City, Zhejiang Province

Patentee before: Xu Qianqian