CN111285623A - Composite aerogel fiber free of powder falling and preparation process thereof - Google Patents

Composite aerogel fiber free of powder falling and preparation process thereof Download PDF

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Publication number
CN111285623A
CN111285623A CN202010288043.XA CN202010288043A CN111285623A CN 111285623 A CN111285623 A CN 111285623A CN 202010288043 A CN202010288043 A CN 202010288043A CN 111285623 A CN111285623 A CN 111285623A
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China
Prior art keywords
aerogel
fiber
water
powder
fibers
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CN202010288043.XA
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Chinese (zh)
Inventor
闫梦祥
杨浩
罗肖宁
常稳
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Henan Aibiaihe New Material Co ltd
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Henan Aibiaihe New Material Co ltd
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Priority to CN202010288043.XA priority Critical patent/CN111285623A/en
Publication of CN111285623A publication Critical patent/CN111285623A/en
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    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL 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
    • C03C25/00—Surface treatment of fibres or filaments made from glass, minerals or slags
    • C03C25/10—Coating
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    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
    • B01J13/0091—Preparation of aerogels, e.g. xerogels
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  • Chemical Or Physical Treatment Of Fibers (AREA)

Abstract

The invention belongs to the field of aerogel materials, and discloses a composite aerogel fiber free of powder falling and a preparation process thereof, which are used for solving the problem that the conventional aerogel is easy to powder fall. The composite aerogel fiber without powder falling comprises aerogel fiber and a water-based adhesive layer, wherein the water-based adhesive layer is wrapped outside the aerogel fiber. The preparation method comprises the following steps: the method comprises the steps of firstly preparing aerogel fibers, then enabling the aerogel fibers to pass through a water-soaking adhesive in a spinning mode to coat water-based glue on the fibers, and then drying and rolling the fibers through a drying channel. Or extruding the glue into a cylinder in an extrusion mode, and drawing the aerogel fibers out of the cylinder through one piece. The invention adopts the water-based adhesive to form a film to encapsulate the aerogel fibers, so as to prepare the aerogel fibers without powder dropping, thereby greatly preventing the occurrence of the condition of the powder dropping of the fibers, completely eradicating the condition that the heat preservation of the aerogel adhesive tape is invalid, prolonging the service life of the aerogel fibers, and the aerogel adhesive tape woven by the fibers without powder dropping has good air permeability and excellent heat preservation performance.

Description

Composite aerogel fiber free of powder falling and preparation process thereof
Technical Field
The invention belongs to the field of aerogel materials, and particularly relates to a composite aerogel fiber free of powder falling and a preparation process thereof.
Background
The aerogel is a nanometer advanced material with a three-dimensional network structure, and the medium filled in the spatial network structure of the aerogel is air, so the aerogel has excellent performances of extremely low density, low heat conductivity coefficient, high porosity and the like, and has very wide application prospects in the fields of heat preservation, heat insulation, energy conservation and consumption reduction.
The aerogel fabric has the excellent performances of low heat conductivity coefficient, air permeability, heat preservation and the like, and can be made into aerogel clothes. Compared with the traditional clothes, the aerogel clothes with the same heat preservation performance are thinner, so that people need to wear more traditional clothes to meet the requirement of keeping warm when the temperature is lower, but the clothes which are too bulky affect the appearance and are heavy. The aerogel clothes can meet the requirement of keeping warm only by being very thin, so that people can keep good stature in cold winter. The existing aerogel clothes have the defects of easy powder falling and incapability of being washed by water.
Disclosure of Invention
In order to overcome the defects described in the prior art, the invention provides the composite aerogel fiber without powder falling and the preparation process thereof in order to realize the preparation of the aerogel clothes without powder falling from the composite aerogel fiber.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows:
the composite aerogel fiber without falling powder comprises aerogel fiber and a water-based adhesive layer, wherein the water-based adhesive layer is wrapped outside the aerogel fiber.
As a preferred scheme of the invention, the aerogel fiber has a diameter of 0.01mm-3mm, and comprises aerogel powder and fiber, wherein the weight part ratio of the aerogel powder to the fiber is 1-60 parts of aerogel powder required by 100 parts of fiber.
In a preferred embodiment of the present invention, the fiber is one of a pre-oxidized fiber, a glass fiber, a carbon fiber, a basalt fiber, a PP fiber, a ceramic fiber, a mullite fiber, a polyurethane fiber, and a PET fiber.
As a preferable scheme of the invention, the aerogel powder comprises SiO2Aerogel powder, TiO2Aerogel powder, AL2O3Aerogel powders, Li2One or more of O aerogel powder, graphene aerogel powder, carbon aerogel powder, polyurethane aerogel powder, zirconia aerogel powder and the like, wherein the particle size range of the aerogel powder is 80-900 meshes.
As a preferable scheme of the invention, the thickness of the water-based adhesive layer is 0.01mm-3 mm; the adhesive comprises a water-based adhesive, wherein the water-based adhesive comprises one of an epoxy resin adhesive, an acrylic adhesive, an acrylate adhesive, an EVA adhesive, a polyester adhesive, a polyether adhesive, a polyurethane adhesive, a polyurea adhesive and the like.
A preparation process of a composite aerogel fiber without powder falling comprises the following steps:
(1) aerogel fibers were prepared.
The method comprises the following specific steps:
(a) preparing hydrolysate; the silicon content and the ethanol content in the hydrolysate are proportioned according to the volume ratio of silicon: ethanol =1:5-40, then adding a catalyst for catalytic hydrolysis, wherein the hydrolysis temperature is 30-100 ℃.
(b) Dipping fibers in glue;
performing sol, and soaking the fiber in the sol for 20-180 min.
(c) Aging;
and (5) carrying out gel aging at room temperature for 5-36 h.
(d) Drying;
the drying is CO2Supercritical drying with CO2Supercritical drying, CO2The pressure is 12MPa, the temperature is 30-100 ℃, and the drying time is 2-12 h. Other drying methods, such as drying under atmospheric pressure and freeze drying, which achieve the same drying effect, can also be used.
(2) And preparing the water-based adhesive.
The water-based adhesive and water are mixed according to the proportion that the water-based adhesive is: water =1:1-10.
(3) And (6) coating glue.
And (3) putting the prepared aerogel fiber into a water-based adhesive, and then drawing out or extruding the aerogel fiber to remove the redundant water-based adhesive.
(4) And (5) drying.
And (3) directly passing the extracted or extruded aerogel fiber filaments through a drying tunnel, wherein the temperature of the drying tunnel is 25-150 ℃, and the drying time is 1-20 min. Drying the water-based adhesive into a glue film to be coated on the aerogel fiber to form the aerogel fiber without powder falling.
(5) And (6) rolling.
Collecting the dried aerogel fiber without powder falling in a rolling mode.
As a preferable scheme of the invention, the application of the composite aerogel fiber without powder falling on the fabric can be made into aerogel clothes, aerogel tents, aerogel fabrics and other heat-insulating and heat-preserving products.
The invention adopts the mode that the water-based adhesive forms a film to encapsulate the aerogel fibers, so that the aerogel fibers without powder falling are prepared, the occurrence of the condition of fiber powder falling can be greatly prevented, the condition that the heat preservation of the aerogel adhesive tape is invalid is avoided, the service life of the aerogel fibers is prolonged, and the aerogel adhesive tape woven by the fibers without powder falling has good air permeability and excellent heat preservation performance.
The powder-falling-free aerogel fibers used in the invention have the advantages of simple manufacturing process, wide application and the like, the fibers belong to upstream products, most downstream products of the fibers can be replaced by the powder-falling-free aerogel fibers, and the application is wide.
Detailed Description
The technical solutions in the embodiments of the present invention are 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 obtained by a person skilled in the art without inventive effort based on the embodiments of the present invention, are within the scope of the present invention.
Example 1:
the composite aerogel fiber without falling powder comprises aerogel fiber and a water-based adhesive layer, wherein the water-based adhesive layer is wrapped outside the aerogel fiber.
In this embodiment, the diameter of the aerogel fiber is 0.01mm to 3mm, and the aerogel fiber includes aerogel powder and fiber, and the weight ratio of the aerogel powder to the fiber is 1 to 60 parts per 100 parts of the aerogel powder required by the fiber.
The fiber is one of pre-oxidized fiber, glass fiber, carbon fiber, basalt fiber, PP fiber, ceramic fiber, mullite fiber, polyurethane fiber and PET fiber.
The particle size of the aerogel powder is 80-900 meshes and comprises SiO2Aerogel powder, TiO2Aerogel powder, AL2O3Aerogel powders, Li2One or more of O aerogel powder, graphene aerogel powder, carbon aerogel powder, polyurethane aerogel powder, zirconia aerogel powder and the like, and aerogel powder.
The thickness of the water-based adhesive layer is 0.01mm-3 mm; the adhesive comprises a water-based adhesive, wherein the water-based adhesive comprises one of an epoxy resin adhesive, an acrylic adhesive, an acrylate adhesive, an EVA adhesive, a polyester adhesive, a polyether adhesive, a polyurethane adhesive, a polyurea adhesive and the like.
Example 2:
a preparation process of a composite aerogel fiber without powder falling comprises the following steps:
(1) aerogel fibers were prepared.
The method comprises the following specific steps:
(a) preparing hydrolysate; silicon content: ethanol (volume ratio) =1:5-40, then catalyst is added for catalytic hydrolysis, and the hydrolysis temperature is 30-100 ℃.
(b) Dipping fibers in glue;
performing sol, and soaking the fiber in the sol for 20-180 min.
(c) Aging;
and (5) carrying out gel aging at room temperature for 5-36 h.
(d) Drying;
the drying is CO2Supercritical drying with CO2Supercritical drying, CO2The pressure is 12MPa, the temperature is 30-100 ℃, and the time is 2-12 h. Other drying methods, such as drying under atmospheric pressure and freeze drying, can also be used to achieve the same effect.
(2) And preparing the water-based adhesive.
The water-based adhesive and water are mixed according to the proportion that the water-based adhesive is: water =1:1-10.
(3) Coating glue;
and (3) putting the prepared aerogel fiber into a water-based adhesive, and then drawing out or extruding the aerogel fiber to remove the redundant water-based adhesive.
The drawing out of the aerogel fibers is to pass the aerogel fibers through a water-based adhesive in a silk drawing mode.
The extruded aerogel fiber is formed by extruding glue into a cylinder and drawing the aerogel fiber out of the cylinder through one block.
(4) Drying;
and (3) directly passing the extracted or extruded aerogel fiber filaments through a drying tunnel, wherein the temperature of the drying tunnel is 25-150 ℃, and the drying time is 1-20 min. Drying the water-based adhesive into a glue film to be coated on the aerogel fiber to form the aerogel fiber without powder falling.
(5) Rolling;
collecting the dried aerogel fiber without powder falling in a rolling mode.
The vibration mass loss rate of the aerogel fibers prepared by the traditional process and the non-dusting fibers prepared by the process is tested to verify the dusting prevention performance of the preparation process.
The method comprises the following steps: 100mm x 100mm of the sample prepared by the traditional process and 100mm x 100mm of the sample prepared by the process of the invention are respectively placed in a standard test sieve with the aperture of 0.250mm, and the vibration frequency of 1400 times/minute and the amplitude of 3mm are set for 5 min. Tests show that the vibration mass loss rate of the sample prepared by the traditional process is 0.5-5%, and the vibration mass loss rate of the non-dusting fiber prepared by the process is 0.05-0.3%, so that the effect brought by the preparation process disclosed by the invention is greatly superior to that of the traditional process, and the aerogel fiber prepared by the process disclosed by the invention is non-dusting.
Example 2:
the application of the composite aerogel fiber without powder falling on the fabric can be made into aerogel clothes, aerogel tents, aerogel fabrics and other heat-insulating products.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are included in the scope of the present invention.

Claims (10)

1. The utility model provides a compound aerogel fibre that does not fall powder which characterized in that: comprises aerogel fibers and a water-based adhesive layer, wherein the water-based adhesive layer is wrapped outside the aerogel fibers.
2. A non-dusting composite aerogel fiber as claimed in claim 1, wherein: the aerogel fiber comprises aerogel powder and fiber, wherein the aerogel powder and the fiber are mixed according to the weight part ratio of 1-60 parts of aerogel powder required by every 100 parts of fiber.
3. Non-dusting composite aerogel fibers according to claim 1 or 2, characterized in that: the diameter of the aerogel fiber is 0.01mm-3 mm.
4. The non-dusting composite aerogel fiber of claim 2, wherein: the fiber is one of pre-oxidized fiber, glass fiber, carbon fiber, basalt fiber, PP fiber, ceramic fiber, mullite fiber, polyurethane fiber and PET fiber.
5. The non-dusting composite aerogel fiber of claim 2, wherein: the aerogel powder comprises SiO2Aerogel powder, TiO2Aerogel powder, AL2O3Aerogel powders, Li2One or more of O aerogel powder, graphene aerogel powder, carbon aerogel powder, polyurethane aerogel powder and zirconia aerogel powder, wherein the granularity of the aerogel powder ranges from 80 meshes to 900 meshes.
6. A non-dusting composite aerogel fiber as claimed in claim 1, wherein: the water-based adhesive layer comprises a water-based adhesive, and the water-based adhesive comprises one of an epoxy resin adhesive, an acrylic adhesive, an acrylate adhesive, an EVA adhesive, a polyester adhesive, a polyether adhesive, a polyurethane adhesive and a polyurea adhesive.
7. Non-dusting composite aerogel fibers according to claim 1 or 6, characterized in that: the thickness of the water-based adhesive layer is 0.01mm-3 mm.
8. A preparation process of a composite aerogel fiber without powder falling is characterized by comprising the following steps:
(1) preparing aerogel fibers by the steps of;
(a) preparing hydrolysate; (b) dipping fibers in glue; (c) aging; (d) drying; the drying is CO2Supercritical drying or normal pressure drying or freeze drying;
(2) preparing a water-based adhesive;
the water-based adhesive and water are mixed according to the proportion that the water-based adhesive is: water =1: 1-10;
(3) coating glue;
putting the prepared aerogel fiber into a water-based adhesive, then drawing out or extruding the aerogel fiber, and removing the redundant water-based adhesive;
(4) drying;
directly passing the extracted or extruded aerogel fiber through a drying tunnel, wherein the temperature of the drying tunnel is 25-150 ℃, and the drying time is 1-20 min; drying the water-based adhesive into a glue film to be coated on the aerogel fiber to form the aerogel fiber without powder falling;
(5) rolling;
collecting the dried aerogel fiber without powder falling in a rolling mode.
9. The process for preparing non-dusting composite aerogel fibers according to claim 8, wherein the specific steps of preparing aerogel fibers are as follows: (a) preparing hydrolysate;
the silicon content and the ethanol content in the hydrolysate are proportioned according to the volume ratio of silicon: ethanol =1:5-40, then adding a catalyst for catalytic hydrolysis, wherein the hydrolysis temperature is 30-100 ℃;
(b) dipping fibers in glue;
performing sol, and soaking the fiber in the sol for 20-180 min;
(c) aging;
gelling and aging at room temperature for 5-36 h;
(d) drying;
the drying is CO2Supercritical drying with CO2Supercritical drying, CO2The pressure is 5MPa-20MPa, the temperature is 30-100 ℃, and the time is 2-12 h.
10. Use of a non-dusting composite aerogel fiber according to any of claims 1-9 on a fabric.
CN202010288043.XA 2020-04-14 2020-04-14 Composite aerogel fiber free of powder falling and preparation process thereof Pending CN111285623A (en)

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