CN110539536B - Lightweight silica aerogel composite thermal insulation fabric and preparation method thereof - Google Patents
Lightweight silica aerogel composite thermal insulation fabric and preparation method thereof Download PDFInfo
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- CN110539536B CN110539536B CN201910782729.1A CN201910782729A CN110539536B CN 110539536 B CN110539536 B CN 110539536B CN 201910782729 A CN201910782729 A CN 201910782729A CN 110539536 B CN110539536 B CN 110539536B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
- B32B37/12—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by using adhesives
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B5/00—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts
- B32B5/22—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed
- B32B5/24—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed one layer being a fibrous or filamentary layer
- B32B5/26—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed one layer being a fibrous or filamentary layer another layer next to it also being fibrous or filamentary
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B7/00—Layered products characterised by the relation between layers; Layered products characterised by the relative orientation of features between layers, or by the relative values of a measurable parameter between layers, i.e. products comprising layers having different physical, chemical or physicochemical properties; Layered products characterised by the interconnection of layers
- B32B7/04—Interconnection of layers
- B32B7/12—Interconnection of layers using interposed adhesives or interposed materials with bonding properties
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2260/00—Layered product comprising an impregnated, embedded, or bonded layer wherein the layer comprises an impregnation, embedding, or binder material
- B32B2260/02—Composition of the impregnated, bonded or embedded layer
- B32B2260/021—Fibrous or filamentary layer
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2262/00—Composition or structural features of fibres which form a fibrous or filamentary layer or are present as additives
- B32B2262/02—Synthetic macromolecular fibres
- B32B2262/0246—Acrylic resin fibres
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2262/00—Composition or structural features of fibres which form a fibrous or filamentary layer or are present as additives
- B32B2262/02—Synthetic macromolecular fibres
- B32B2262/0261—Polyamide fibres
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2262/00—Composition or structural features of fibres which form a fibrous or filamentary layer or are present as additives
- B32B2262/04—Cellulosic plastic fibres, e.g. rayon
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2307/00—Properties of the layers or laminate
- B32B2307/30—Properties of the layers or laminate having particular thermal properties
- B32B2307/304—Insulating
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2307/00—Properties of the layers or laminate
- B32B2307/50—Properties of the layers or laminate having particular mechanical properties
- B32B2307/554—Wear resistance
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2307/00—Properties of the layers or laminate
- B32B2307/70—Other properties
- B32B2307/732—Dimensional properties
- B32B2307/734—Dimensional stability
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2437/00—Clothing
Landscapes
- Chemical Or Physical Treatment Of Fibers (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
The invention relates to the field of fabrics, in particular to a lightweight silica aerogel composite thermal insulation fabric and a preparation method thereof. The utility model provides a lightweight silica aerogel composite insulation surface fabric, includes the wear-resisting protection precoat on top layer, the heat preservation insulating layer in intermediate level and the comfortable precoat next to the shin of inlayer at least, and the material on wear-resisting protection precoat is the polyamide fibre, and the material on heat preservation insulating layer is silica aerogel/viscose combined material, and the material on the comfortable precoat next to the shin is acrylic fiber. By combining the technical means of selecting viscose fibers with specific sizes and modifying the silicon dioxide aerogel/viscose fiber composite material by adopting a silane coupling agent containing carboxyl and the like, the water washing resistance and shrinkage resistance of the composite material are effectively improved, and the light weight and heat preservation effect of the composite fabric are further ensured.
Description
Technical Field
The invention relates to the field of fabrics, in particular to a lightweight silica aerogel composite thermal insulation fabric and a preparation method thereof.
Background
With the development of science and technology and the progress of society, the requirements of people on the quality of life are higher and higher, and the textile extends from the function of resisting cold of the traditional shield to the functions of beauty, comfort, portability and the like. With the development of the consumption concept of people, various intelligent and functional fabrics are widely concerned and developed. In recent years, various modified composite thermal insulation materials such as washing cotton, shaped degreasing washing cotton, down wadding felt, wool fabric, composite needling, melt-blown cotton and other thermal insulation materials continuously appear, and new technology, new process and new equipment continuously appear, so that the traditional thermal insulation materials are improved and researched, the advantages and the disadvantages are improved, the technical content is improved, and the comprehensive performance is improved.
The aerogel is considered to be the lightest material in the world due to the unique three-dimensional nano-scale pore structure and extremely low density and heat conductivity coefficient, can be used as a raw material for gas filtration and can also be prepared into a heat insulation material. The most common aerogel is silicon dioxide aerogel, but because the skeleton forming a silicon dioxide aerogel network structure is thin, and the acting force between secondary particles of the silicon dioxide aerogel is weak, the secondary particles of the silicon dioxide aerogel have the defects of easy water absorption, poor toughness and the like, so the secondary particles can not be used independently, and the multifunctional aerogel can be prepared by compounding with other materials (such as glass fiber, viscose fiber, resin and the like), has the excellent characteristics of the aerogel, and can be widely applied to the fields of fabrics, medicines, military industry, aerospace, navigation, high-speed rail, paper making and the like.
However, when the silica aerogel and the viscose fiber are compounded, the prepared light heat-preservation fabric has the defects of poor toughness, poor water washing resistance, poor dimensional stability after long-time repeated water washing and the like, and in addition, the composite fabric is easy to absorb moisture and has serious shrinkage, so that the prepared silica aerogel composite material has poor heat insulation and heat preservation performance.
Disclosure of Invention
In order to solve the technical problems, the invention provides a lightweight silica aerogel composite thermal insulation fabric which at least comprises a wear-resistant protective fabric layer on a surface layer, a thermal insulation layer on a middle layer and a close-fitting comfortable fabric layer on an inner layer, wherein the wear-resistant protective fabric layer is made of nylon, the thermal insulation layer is made of a silica aerogel/viscose composite material, and the close-fitting comfortable fabric layer is made of acrylic.
As a preferable technical scheme of the invention, the wear-resistant protective fabric layer and the heat-insulating layer, and the heat-insulating layer and the close-fitting comfortable fabric layer are adhered together through adhesives.
In a preferred embodiment of the present invention, the adhesive is a silicone resin adhesive.
In a preferred embodiment of the present invention, the cut length of the viscose fiber is 35 to 40mm, and the fineness of the viscose fiber is 1.0 to 2.5 denier.
In a preferred embodiment of the present invention, the cut length of the viscose fiber is 36.5 to 38.5mm, and the fineness of the viscose fiber is 1.2 to 2.0 denier.
As a preferred technical solution of the present invention, the silica aerogel/viscose fiber composite material is a silane coupling agent modified silica aerogel/viscose fiber composite material.
In a preferred embodiment of the present invention, the silane coupling agent is a silane coupling agent containing a carboxyl group.
As a preferred technical solution of the present invention, the preparation method of the silica aerogel/viscose fiber composite material comprises the following steps:
(1) mixing ethyl orthosilicate, water and ethanol according to a molar ratio of 1 (3-7) to (6-10), adding 0.05-0.25 mol/L oxalic acid solution into the precursor solution, adjusting the pH value of the solution to 3-4.5, stirring for 20-40 min, taking out the mixed solution, placing the mixed solution in a water bath kettle for constant-temperature hydrolysis for 13-18 h, adding 0.45-0.65 mol/L ammonia water solution, adjusting the pH value to 7-8, stirring, and standing to obtain silica sol;
(2) sizing viscose fibers by using a mold to obtain a fiber prefabricated part, vacuumizing and dipping silica sol, sealing and storing to obtain gel 1, placing the gel 1 in an ethanol solution for aging for 10-13 h, and exchanging a solvent for 1-2.5 d to obtain gel 2;
(3) and (3) carrying out surface treatment on the gel 2 by adopting a solution with the molar ratio of n-hexane to the silane coupling agent being 1 (2-8), washing away residual modification liquid by using n-hexane, and drying at normal pressure to obtain the modified hydrogel.
According to a preferable technical scheme, the mass ratio of the silicon dioxide aerogel/viscose fiber composite material to the silane coupling agent is 1 (1-6).
The second aspect of the invention provides a preparation method of a lightweight silica aerogel composite thermal insulation fabric, which comprises the following steps:
(1) firstly, sticking the wear-resistant protective fabric layer of the surface layer and the heat-insulating layer of the middle layer together through an adhesive, and then sticking the heat-insulating layer of the middle layer and the close-fitting comfortable fabric layer of the inner layer together through the adhesive to obtain a fabric 1;
(2) and (3) leading the fabric 1 to pass through a wave head of an ultrasonic sewing machine to enable the fabric surface to generate wave vibration on a pattern roller to form the fabric surface with uniform pressure points, thus obtaining the fabric.
Has the advantages that: the invention provides a portable silicon dioxide aerogel composite heat-insulation fabric and a preparation method thereof, firstly, viscose fibers with specific sizes are selected to be compounded with silicon dioxide aerogel, and the portable heat-insulation fabric is obtained; secondly, the silicon dioxide aerogel/viscose fiber composite material is modified by the silane coupling agent containing carboxyl, so that the combination strength of the silicon dioxide aerogel and the viscose fiber is improved, the toughness and the water absorption performance of the silicon dioxide aerogel are improved, and the three-dimensional network pore structure of the silicon dioxide aerogel is maintained; on the other hand, the phenomenon that the composite material is easy to shrink is improved, and the dimensional stability of the composite material after long-time washing is ensured; in addition, the viscose fibers with specific sizes are selected and the technical means of modifying the composite material by adopting the silane coupling agent containing carboxyl and the like are combined, so that the water washing resistance and the water shrinkage resistance of the composite material are effectively improved, and the light weight and the heat preservation effect of the composite fabric are further ensured.
Detailed Description
The disclosure may be understood more readily by reference to the following detailed description of preferred embodiments of the invention and the examples included therein. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. In case of conflict, the present specification, including definitions, will control.
The term "prepared from …" as used herein is synonymous with "comprising". The terms "comprises," "comprising," "includes," "including," "has," "having," "contains," "containing," or any other variation thereof, as used herein, are intended to cover a non-exclusive inclusion. For example, a composition, process, method, article, or apparatus that comprises a list of elements is not necessarily limited to only those elements but may include other elements not expressly listed or inherent to such composition, process, method, article, or apparatus.
The conjunction "consisting of …" excludes any unspecified elements, steps or components. If used in a claim, the phrase is intended to claim as closed, meaning that it does not contain materials other than those described, except for the conventional impurities associated therewith. When the phrase "consisting of …" appears in a clause of the subject matter of the claims rather than immediately after the subject matter, it defines only the elements described in the clause; other elements are not excluded from the claims as a whole.
When an amount, concentration, or other value or parameter is expressed as a range, preferred range, or as a range of upper preferable values and lower preferable values, this is to be understood as specifically disclosing all ranges formed from any pair of any upper range limit or preferred value and any lower range limit or preferred value, regardless of whether ranges are separately disclosed. For example, when a range of "1 to 5" is disclosed, the described range should be interpreted to include the ranges "1 to 4", "1 to 3", "1 to 2 and 4 to 5", "1 to 3 and 5", and the like. When a range of values is described herein, unless otherwise stated, the range is intended to include the endpoints thereof and all integers and fractions within the range.
The singular forms "a", "an" and "the" include plural referents unless the context clearly dictates otherwise. "optional" or "any" means that the subsequently described event or events may or may not occur, and that the description includes instances where the event occurs and instances where it does not.
Approximating language, as used herein throughout the specification and claims, is intended to modify a quantity, such that the invention is not limited to the specific quantity, but includes portions that are literally received for modification without substantial change in the basic function to which the invention is related. Accordingly, the use of "about" to modify a numerical value means that the invention is not limited to the precise value. In some instances, the approximating language may correspond to the precision of an instrument for measuring the value. In the present description and claims, range limitations may be combined and/or interchanged, including all sub-ranges contained therein if not otherwise stated.
In addition, the indefinite articles "a" and "an" preceding an element or component of the invention are not intended to limit the number requirement (i.e., the number of occurrences) of the element or component. Thus, "a" or "an" should be read to include one or at least one, and the singular form of an element or component also includes the plural unless the stated number clearly indicates that the singular form is intended.
In order to solve the technical problems, the invention provides a lightweight silica aerogel composite thermal insulation fabric which at least comprises a wear-resistant protective fabric layer on a surface layer, a thermal insulation layer on a middle layer and a close-fitting comfortable fabric layer on an inner layer, wherein the wear-resistant protective fabric layer is made of nylon, the thermal insulation layer is made of a silica aerogel/viscose fiber composite material, and the close-fitting comfortable fabric layer is made of acrylic.
Silicone resin
The organic silicon resin (also called polysiloxane) is a general name of a polymer which is formed by alternately connecting silicon atoms and oxygen atoms to form a framework, and different organic groups are connected with the silicon atoms; the organic silicon resin structure contains both organic groups and inorganic structures, and the special composition and molecular structure make the organic silicon resin integrate the characteristics of organic matters and the functions of inorganic matters.
In a preferred embodiment, the silicone resin of the present invention is selected from one or more of polyalkyl silicone resins, polyaryl silicone resins and polyalkyl aryl silicone resins.
As examples of polyalkyl silicone resins, include, but are not limited to: polymethyl silicone resin and polyethyl silicone resin.
In a most preferred embodiment, the silicone resin of the present invention is model BD-833, available from New Material science, Inc. of Border, Hangzhou.
Nylon
The nylon of the invention is also called nylon and nylon, is the trade name of Polyamide fiber, the English name is polyamine (PA for short), and the density is 1.15g/cm3The basic composition substance is through amido bond [ NHCO]The linked aliphatic polyamides are produced in large quantities and are widely used, the designation of which is determined by the specific number of carbon atoms of the synthetic monomers.
In a preferred embodiment, the nylon of the invention is selected from one or more of nylon 6, nylon 66, nylon 11 and nylon 610.
In a most preferred embodiment, the polyamide of the present invention is polyamide 66, available from Hengyi Dai composites, Inc. of Zhejiang.
Acrylic fibre
The acrylic fiber is the trade name of polyacrylonitrile in China, called as "Orlon" and "keslen" abroad, and called as Orlon by DuPont in America, is an important raw material for wool spinning industry, is also an important variety of synthetic fiber, and can be blended with wool, terylene, viscose and cotton to prepare various exquisite fabrics, artificial furs and industrial products.
In a preferred embodiment, the acrylic fibers of the present invention were purchased from Weichaft Fund textile Co., Ltd.
Viscose fiber
The viscose fiber is cellulose fiber obtained by taking 'wood' as a raw material and extracting and remolding fiber molecules from natural wood cellulose; the cotton yarn has the characteristics of smoothness, coolness, ventilation, static resistance, ultraviolet resistance, gorgeous color, good dyeing fastness and the like, and also has the characteristics of cotton essence, silk quality and the like; is a genuine plant fiber which is from nature and is superior to nature; the fabric is widely applied to the fields of various underwear, textile, clothes, non-woven fabrics and the like.
In a preferred embodiment, the viscose fiber of the present invention has a cut length of 35 to 40mm and a fineness of 1.0 to 2.5 denier.
In a more preferred embodiment, the viscose fiber of the present invention has a cut length of 36.5 to 38.5mm and a fineness of 1.2 to 2.0 denier.
In a most preferred embodiment, the viscose fibers of the invention have a staple length of 37.5mm and a denier of 1.5 denier, available from Zhongtai chemical.
Silica aerogel
The silicon dioxide aerogel is a nano porous amorphous material with a nano porous three-dimensional network structure formed by mutually gathering nano-scale colloidal particles and gas media filled in pores of the nano porous three-dimensional network structure.
Silica aerogel/viscose composite
The silicon dioxide aerogel/viscose fiber composite material is a silicon dioxide aerogel/viscose fiber composite material modified by a silane coupling agent.
In a preferred embodiment, the silane coupling agent of the present invention is a silane coupling agent containing a carboxyl group.
In a more preferred embodiment, the silane coupling agent of the present invention is a silane coupling agent containing a carboxyl group.
In a most preferred embodiment, the silane coupling agent containing a carboxyl group according to the present invention is 1, 3-bis (3-carboxypropyl) tetramethyldisiloxane (CAS: 3353-68-2).
In a preferred embodiment, the preparation method of the modified silica aerogel/viscose fiber composite material of the present invention comprises the following steps:
(1) mixing ethyl orthosilicate, water and ethanol according to a molar ratio of 1 (3-7) to (6-10), adding 0.05-0.25 mol/L oxalic acid solution into the precursor solution, adjusting the pH value of the solution to 3-4.5, stirring for 20-40 min, taking out the mixed solution, placing the mixed solution in a water bath kettle for constant-temperature hydrolysis for 13-18 h, adding 0.45-0.65 mol/L ammonia water solution, adjusting the pH value to 7-8, stirring, and standing to obtain silica sol;
(2) sizing viscose fibers by using a mold to obtain a fiber prefabricated part, vacuumizing and dipping silica sol, sealing and storing to obtain gel 1, placing the gel 1 in an ethanol solution for aging for 10-13 h, and exchanging a solvent for 1-2.5 d to obtain gel 2;
(3) and (3) carrying out surface treatment on the gel 2 by adopting a solution with the molar ratio of n-hexane to the silane coupling agent being 1 (2-8), washing away residual modification liquid by using n-hexane, and drying at normal pressure to obtain the modified hydrogel.
In a more preferred embodiment, the method for preparing the modified silica aerogel/viscose fiber composite material according to the present invention comprises the following steps:
(1) mixing ethyl orthosilicate, water and ethanol according to a molar ratio of 1 (4-6) to (7-9), adding 0.1-0.2 mol/L oxalic acid solution into the precursor solution, adjusting the pH value of the solution to 3-4.5, stirring for 25-35 min, taking out the mixed solution, placing the mixed solution in a water bath kettle for hydrolysis at a constant temperature for 14-17 h, adding 0.5-0.6 mol/L ammonia water solution, adjusting the pH value to 7-8, stirring, and standing to obtain silica sol;
(2) sizing viscose fibers by using a mold to obtain a fiber prefabricated part, vacuumizing and dipping silica sol, sealing and storing to obtain gel 1, placing the gel 1 in an ethanol solution for aging for 11-12 h, and exchanging a solvent for 1.5-2 d to obtain gel 2;
(3) and (3) carrying out surface treatment on the gel 2 by adopting a solution with the molar ratio of n-hexane to the silane coupling agent being 1 (3-7), washing away residual modification liquid by using n-hexane, and drying at normal pressure to obtain the modified hydrogel.
In a most preferred embodiment, the method for preparing the modified silica aerogel/viscose fiber composite of the present invention comprises the steps of:
(1) mixing ethyl orthosilicate, water and ethanol according to a molar ratio of 1:5:8, adding 0.15mol/L oxalic acid solution into the precursor solution, adjusting the pH value of the solution to 3-4.5, stirring for 30min, taking out the mixed solution, placing the mixed solution into a water bath kettle, hydrolyzing for 15.5h at a constant temperature, adding 0.55mol/L ammonia water solution, adjusting the pH value to 7-8, stirring, and standing to obtain silica sol;
(2) sizing the viscose fiber by using a mold to obtain a fiber prefabricated part, vacuumizing and dipping silica sol, sealing and storing to obtain gel 1, placing the gel 1 in an ethanol solution for aging for 11.5h, and exchanging a solvent for 1.6d to obtain gel 2;
(3) and (3) carrying out surface treatment on the gel 2 by adopting a solution with the molar ratio of n-hexane to the silane coupling agent being 1:5, washing away residual modification liquid by using n-hexane, and drying at normal pressure to obtain the modified hydrogel.
The mass ratio of the silicon dioxide aerogel/viscose fiber composite material to the silane coupling agent is 1 (1-6).
In a preferred embodiment, the mass ratio of the silica aerogel/viscose composite material to the silane coupling agent is 1 (2-4).
In a most preferred embodiment, the silica aerogel/viscose composite of the present invention and the silane coupling agent are present in a mass ratio of 1: 3.
The inventor of the application finds that the toughness and the glycidyl property of the composite material are effectively improved by modifying the silica aerogel/viscose fiber composite material by using 1, 3-bis (3-carboxypropyl) tetramethyldisiloxane, and probably because hydroxyl formed by hydrolyzing the 1, 3-bis (3-carboxypropyl) tetramethyldisiloxane can form covalent bonds with polar groups on the surface of the aerogel and is grafted with hydrophobic groups, so that the collapse of a pore structure of the aerogel is effectively prevented, and the mechanical property is improved; moreover, the viscose fiber with a specific size is compounded with the silicon dioxide aerogel, and the viscose fiber has more excellent functions of supporting the aerogel Si-O-Si structure and connecting aerogel nanoparticles; the carboxyl of the 1, 3-bis (3-carboxypropyl) tetramethyldisiloxane can also perform chemical reaction with polar groups on the surface of the viscose fiber, so that the loading strength of the silica aerogel on the surface of the viscose fiber is effectively enhanced, and the toughness of the silica aerogel is also enhanced; therefore, the synergistic effect of the 1, 3-bis (3-carboxypropyl) tetramethyldisiloxane and the viscose effectively improves the mechanical property of the silicon dioxide aerogel. In addition, the inventor of the present application further finds that under the conditions that the cut length of the viscose fiber is 35-40 mm and the fineness is 1.0-2.5 denier, the problem of water shrinkage of the composite material after multiple times of washing is effectively solved through the 1, 3-bis (3-carboxypropyl) tetramethyldisiloxane modified composite material, which may be caused by that the carboxyl in the 1, 3-bis (3-carboxypropyl) tetramethyldisiloxane is polymerized with the hydrophilic group in the viscose fiber macromolecules, so that the uniformity of the cross-sectional structure of the viscose fiber is improved, the crystallinity and the orientation of the fiber skin layer and the core layer are relatively balanced, and the shrinkage degree of the viscose fiber is further reduced; meanwhile, the fibers with the length of 35-40 mm and the fineness of 1.0-2.5 deniers are selected, so that the internal stress applied to the viscose fibers and the silicon dioxide aerogel during compounding tends to be in a balanced state, and the shrinkage of the composite material is further relieved from the mechanical angle; in addition, experiments prove that the performance of the silicon dioxide aerogel/viscose fiber composite material is best when the mass ratio of the silicon dioxide aerogel/viscose fiber composite material to the 1, 3-bis (3-carboxypropyl) tetramethyldisiloxane is 1 (1-6).
The second aspect of the invention provides a preparation method of a lightweight silica aerogel composite thermal insulation fabric, which comprises the following steps:
(1) firstly, sticking the wear-resistant protective fabric layer of the surface layer and the heat-insulating layer of the middle layer together through an adhesive, and then sticking the heat-insulating layer of the middle layer and the close-fitting comfortable fabric layer of the inner layer together through the adhesive to obtain a fabric 1;
(2) and (3) leading the fabric 1 to pass through a wave head of an ultrasonic sewing machine to enable the fabric surface to generate wave vibration on a pattern roller to form the fabric surface with uniform pressure points, thus obtaining the fabric.
Examples
Example 1
Embodiment 1 provides a lightweight silica aerogel composite insulation surface fabric, at least includes the wear-resisting protection precoat on top layer, the thermal insulation layer in intermediate level and the comfortable precoat next to the shin of inlayer, the material on wear-resisting protection precoat is the polyamide fibre, the material on thermal insulation layer is silica aerogel/viscose combined material, the material on the comfortable precoat next to the shin is acrylic fibre.
The wear-resistant protective fabric layer and the heat-insulating layer as well as the heat-insulating layer and the close-fitting comfortable fabric layer are adhered together through an adhesive.
The nylon is nylon 66.
The cut length of the viscose fiber is 37.5mm, and the fineness of the viscose fiber is 1.5 deniers.
The silicon dioxide aerogel/viscose fiber composite material is a 1, 3-bis (3-carboxypropyl) tetramethyldisiloxane modified silicon dioxide aerogel/viscose fiber composite material.
In one embodiment, the method for preparing the modified silica aerogel/viscose composite comprises the following steps:
(1) mixing ethyl orthosilicate, water and ethanol according to a molar ratio of 1:5:8, adding 0.15mol/L oxalic acid solution into the precursor solution, adjusting the pH value of the solution to 3-4.5, stirring for 30min, taking out the mixed solution, placing the mixed solution into a water bath kettle, hydrolyzing for 15.5h at a constant temperature, adding 0.55mol/L ammonia water solution, adjusting the pH value to 7-8, stirring, and standing to obtain silica sol;
(2) sizing the viscose fiber by using a mold to obtain a fiber prefabricated part, vacuumizing and dipping silica sol, sealing and storing to obtain gel 1, placing the gel 1 in an ethanol solution for aging for 11.5h, and exchanging a solvent for 1.6d to obtain gel 2;
(3) and (3) carrying out surface treatment on the gel 2 by adopting a solution with the molar ratio of n-hexane to the silane coupling agent being 1:5, washing away residual modification liquid by using n-hexane, and drying at normal pressure to obtain the modified hydrogel.
The mass ratio of the silicon dioxide aerogel/viscose fiber composite material to the 1, 3-bis (3-carboxypropyl) tetramethyldisiloxane is 1: 3.
The preparation method of the lightweight silica aerogel composite thermal insulation fabric comprises the following steps:
(1) firstly, sticking the wear-resistant protective fabric layer of the surface layer and the heat-insulating layer of the middle layer together through an adhesive, and then sticking the heat-insulating layer of the middle layer and the close-fitting comfortable fabric layer of the inner layer together through the adhesive to obtain a fabric 1;
(2) and (3) leading the fabric 1 to pass through a wave head of an ultrasonic sewing machine to enable the fabric surface to generate wave vibration on a pattern roller to form the fabric surface with uniform pressure points, thus obtaining the fabric.
Example 2: the difference from example 1 is that the mass ratio of the silica aerogel/viscose composite to 1, 3-bis (3-carboxypropyl) tetramethyldisiloxane is 1: 0.5.
Example 3: the difference from example 1 is that the mass ratio of the silica aerogel/viscose composite to 1, 3-bis (3-carboxypropyl) tetramethyldisiloxane is 1: 8.
Example 4: the difference from example 1 is that the silica aerogel/viscose fiber composite is an unmodified silica aerogel/viscose fiber composite.
Example 5: the difference from example 1 is that the silica aerogel/viscose fiber composite is a vinyltrichlorosilane modified silica aerogel/viscose fiber composite.
In one embodiment, the method for preparing the modified silica aerogel/viscose composite comprises the following steps:
(1) mixing ethyl orthosilicate, water and ethanol according to a molar ratio of 1:5:8, adding 0.15mol/L oxalic acid solution into the precursor solution, adjusting the pH value of the solution to 3-4.5, stirring for 30min, taking out the mixed solution, placing the mixed solution into a water bath kettle, hydrolyzing for 15.5h at a constant temperature, adding 0.55mol/L ammonia water solution, adjusting the pH value to 7-8, stirring, and standing to obtain silica sol;
(2) sizing the viscose fiber by using a mold to obtain a fiber prefabricated part, vacuumizing and dipping silica sol, sealing and storing to obtain gel 1, placing the gel 1 in an ethanol solution for aging for 11.5h, and exchanging a solvent for 1.6d to obtain gel 2;
(3) and (3) carrying out surface treatment on the gel 2 by adopting a solution with the molar ratio of n-hexane to vinyl trichlorosilane being 1:5, washing away residual modification liquid by using n-hexane, and drying under normal pressure to obtain the modified hydrogel.
Example 6: the difference from example 1 is that the silica aerogel/viscose fiber composite is a vinyltriphenylsilane-modified silica aerogel/viscose fiber composite.
In one embodiment, the method for preparing the modified silica aerogel/viscose composite comprises the following steps:
(1) mixing ethyl orthosilicate, water and ethanol according to a molar ratio of 1:5:8, adding 0.15mol/L oxalic acid solution into the precursor solution, adjusting the pH value of the solution to 3-4.5, stirring for 30min, taking out the mixed solution, placing the mixed solution into a water bath kettle, hydrolyzing for 15.5h at a constant temperature, adding 0.55mol/L ammonia water solution, adjusting the pH value to 7-8, stirring, and standing to obtain silica sol;
(2) sizing the viscose fiber by using a mold to obtain a fiber prefabricated part, vacuumizing and dipping silica sol, sealing and storing to obtain gel 1, placing the gel 1 in an ethanol solution for aging for 11.5h, and exchanging a solvent for 1.6d to obtain gel 2;
(3) and (3) carrying out surface treatment on the gel 2 by adopting a solution with the molar ratio of n-hexane to vinyl triphenylsilane being 1:5, washing away residual modification liquid by using n-hexane, and drying under normal pressure to obtain the modified hydrogel.
Example 7: the difference from example 1 is that the cut length of the viscose fiber is 42mm and the fineness is 0.8 denier.
Example 8: the difference from example 1 is that the viscose fiber has a cut length of 38mm and a fineness of 2.8 denier.
Example 9: the difference from example 1 is that the mass ratio of the silica aerogel/viscose composite to 1, 3-bis (3-carboxypropyl) tetramethyldisiloxane is 1: 0.5; the cut length of the viscose fiber is 42mm, and the fineness of the viscose fiber is 2.8 deniers.
Evaluation of Performance
1. Elongation at break test
The silica aerogel/viscose composites prepared in examples 1 to 9 were tested for elongation at break according to GB/T24218.18-2014.
2. And (3) testing the shrinkage rate:
the silica aerogel/viscose composites prepared in examples 1 to 9 were tested for shrinkage according to GB/T8628.
The test results are shown in table 1 below.
Table 1 performance characterization test
| Elongation at break/% | Shrinkage/% of | |
| Example 1 | 12.5 | 4 |
| Example 2 | 10 | 5 |
| Example 3 | 10.1 | 5.5 |
| Example 4 | 8 | 7 |
| Example 5 | 8.2 | 6.8 |
| Example 6 | 8.3 | 6.5 |
| Example 7 | 11 | 4.5 |
| Example 8 | 10.5 | 4.8 |
| Example 9 | 9 | 7.9 |
As can be seen from table 1, the silica aerogel composite fabric prepared according to the present invention has very good elongation at break and weak water shrinkage. It can be seen from the comparative example that, when the heat preservation fabric simultaneously has: the cut length of the viscose fiber is 35-40 mm, the fineness of the viscose fiber is 1.0-2.5 deniers, and when the viscose fiber passes through the 1, 3-bis (3-carboxypropyl) tetramethyldisiloxane modified silicon dioxide aerogel/viscose fiber sewing material, the performance of the fabric is optimal.
The foregoing examples are merely illustrative and serve to explain some of the features of the method of the present invention. The appended claims are intended to claim as broad a scope as is contemplated, and the examples presented herein are merely illustrative of selected implementations in accordance with all possible combinations of examples. Accordingly, it is applicants' intention that the appended claims are not to be limited by the choice of examples illustrating features of the invention. Also, where numerical ranges are used in the claims, subranges therein are included, and variations in these ranges are also to be construed as possible being covered by the appended claims.
Claims (5)
1. A portable silicon dioxide aerogel composite thermal insulation fabric is characterized by at least comprising a wear-resistant protective fabric layer on a surface layer, a thermal insulation layer on a middle layer and a close-fitting comfortable fabric layer on an inner layer, wherein the wear-resistant protective fabric layer is made of nylon, the thermal insulation layer is made of a silicon dioxide aerogel/viscose composite material, and the close-fitting comfortable fabric layer is made of acrylic fibers;
the silicon dioxide aerogel/viscose fiber composite material is a silicon dioxide aerogel/viscose fiber composite material modified by a silane coupling agent;
the silane coupling agent is 1, 3-bis (3-carboxypropyl) tetramethyldisiloxane (CAS: 3353-68-2);
the preparation method of the modified silicon dioxide aerogel/viscose fiber composite material comprises the following steps:
(1) mixing ethyl orthosilicate, water and ethanol according to a molar ratio of 1 (3-7) to (6-10), adding 0.05-0.25 mol/L oxalic acid solution into the precursor solution, adjusting the pH value of the solution to 3-4.5, stirring for 20-40 min, taking out the mixed solution, placing the mixed solution in a water bath kettle for constant-temperature hydrolysis for 13-18 h, adding 0.45-0.65 mol/L ammonia water solution, adjusting the pH value to 7-8, stirring, and standing to obtain silica sol;
(2) sizing viscose fibers by using a mold to obtain a fiber prefabricated part, vacuumizing and dipping silica sol, sealing and storing to obtain gel 1, placing the gel 1 in an ethanol solution for aging for 10-13 h, and exchanging a solvent for 1-2.5 d to obtain gel 2;
(3) carrying out surface treatment on the gel 2 by adopting a solution with the molar ratio of n-hexane to a silane coupling agent being 1 (2-8), washing away residual modification liquid by using n-hexane, and drying at normal pressure to obtain the modified hydrogel;
the cutting length of the viscose fibers is 35-40 mm, and the fineness of the viscose fibers is 1.0-2.5 deniers;
the mass ratio of the silicon dioxide aerogel/viscose fiber composite material to the silane coupling agent is 1 (1-6).
2. The lightweight silica aerogel composite thermal insulation fabric according to claim 1, wherein the wear-resistant protective fabric layer and the thermal insulation layer, and the thermal insulation layer and the close-fitting comfortable fabric layer are adhered together by adhesives.
3. The lightweight silica aerogel composite insulation fabric according to claim 2, wherein the binder is a silicone resin binder.
4. The lightweight silica aerogel composite thermal insulation fabric according to claim 1, wherein the cut length of the viscose fiber is 36.5-38.5 mm, and the fineness of the viscose fiber is 1.2-2.0 denier.
5. The preparation method of the lightweight silica aerogel composite thermal insulation fabric according to any one of claims 1 to 4, characterized by comprising the following steps: firstly, sticking a wear-resistant protective fabric layer on the surface layer and a heat-insulating layer on the middle layer together through an adhesive, and then sticking the heat-insulating layer on the middle layer and a close-fitting comfortable fabric layer on the inner layer together through the adhesive to obtain a fabric 1; (2) and (3) leading the fabric 1 to pass through a wave head of an ultrasonic sewing machine to enable the fabric surface to generate wave vibration on a pattern roller to form the fabric surface with uniform pressure points, thus obtaining the fabric.
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| CN115852516B (en) * | 2022-12-05 | 2024-04-16 | 江阴市庆丰化纤有限公司 | Heat-preserving heat-insulating antibacterial fiber and preparation method thereof |
| CN117360019B (en) * | 2023-10-24 | 2024-07-16 | 波司登羽绒服装有限公司 | Silicon dioxide aerogel composite heat-insulating fabric and preparation method and application thereof |
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