CN110656443B

CN110656443B - Soft, light, thin and super-thermal aerogel filling material for shoes, clothes, bedding and manufacturing method thereof

Info

Publication number: CN110656443B
Application number: CN201910788876.XA
Authority: CN
Inventors: 白朋
Original assignee: Shenzhen Daimaoniu New Material Technology Co ltd
Current assignee: Jiangsu Da Mao Niu New Material Co.,Ltd.
Priority date: 2019-08-26
Filing date: 2019-08-26
Publication date: 2020-08-11
Anticipated expiration: 2039-08-26
Also published as: CN110656443A

Abstract

The invention relates to the field of shoe, clothes and home furnishing, in particular to a soft, light, thin and super-thermal aerogel filling material for shoes, clothes, bedding and a manufacturing method thereof. The soft, light and thin super-warm aerogel filling material for the bedding and the shoes is prepared by processing non-woven fabrics and glue solution, wherein the raw materials of the non-woven fabrics are selected from profiled fibers and round fibers, and the raw materials of the glue solution at least comprise SiO₂The filling material prepared by dipping the non-woven fabric into the glue solution and then performing a water foaming process has good heat retention, air permeability, moisture permeability and durability.

Description

Soft, light, thin and super-thermal aerogel filling material for shoes, clothes, bedding and manufacturing method thereof

Technical Field

The invention relates to the field of shoe, clothes and home furnishing, in particular to a soft, light, thin and super-thermal aerogel filling material for shoes, clothes, bedding and a manufacturing method thereof.

Background

Shoes, clothes, bedding and the like are necessities of life of people and are indispensable in cold winter. With the improvement of living standard, people have higher requirements on cold-proof and warm-keeping articles, particularly clothes, consumers have requirements on warm keeping, comfort and attractive appearance, and therefore, the novel warm-keeping articles which are soft, light, thin, warm-keeping and breathable are favored.

The traditional cold-proof and warm-keeping articles mostly adopt cotton, hemp, down feather, plush and the like as filling materials, and are thickened or weighted to increase the warm-keeping effect, so that the flexibility of people is limited.

Disclosure of Invention

In order to solve the technical problems, the invention provides a soft, light, thin and super-thermal aerogel filling material for shoes, clothes, bedding and mattress, wherein the filling material is prepared by processing non-woven fabrics and glue solution;

the raw material of the non-woven fabric comprises at least one of profiled fiber and round fiber;

the raw material of the glue solution comprises SiO₂Aerogel, organic solvent.

As a preferred technical scheme of the invention, the raw materials of the non-woven fabric are triangular profiled fibers and round fibers;

the mass ratio of the triangular profiled fibers to the round fibers is (1-4): 8.

as a preferable technical scheme of the invention, the glue solution also comprises an adhesive as a raw material.

As a preferred technical solution of the present invention, the adhesive is an epoxy group-containing polyether polyurethane dispersion;

the particle size of the polyether polyurethane dispersoid containing the epoxy group is 50-100 nm.

As a preferable technical scheme of the invention, the SiO₂The aperture of the aerogel is 20-30 nm.

As a preferable technical scheme of the invention, the raw material of the glue solution also comprises a dispersing agent.

As a preferable technical scheme, the dispersing agent is a compound of sodium polyacrylate and maleic acid-acrylic acid copolymer.

As a preferable technical scheme of the invention, the mass of the maleic acid-acrylic acid copolymer in the compound is not less than 5% of the mass of the sodium polyacrylate.

The invention provides a manufacturing method of a soft, light, thin and super-thermal aerogel filling material for shoes, clothes, bedding and the like, which comprises the following steps:

s1, preparing non-woven fabrics from the profiled fibers and/or the round fibers in a machine cloth mode;

s2, dispersing the raw materials of the glue solution in an organic solvent to obtain the glue solution;

s3, dipping the non-woven fabric in the S1 into the glue solution in the S2, taking out the non-woven fabric after dipping, and obtaining the SiO-carrying fabric₂A nonwoven fabric of aerogel;

s4, carrying SiO in S3₂And placing the non-woven fabric of the aerogel in a coagulating bath, foaming with water, airing, and correcting to obtain the filling material.

As a preferred embodiment of the present invention, the coagulation bath further comprises a catalyst;

the catalyst is tertiary amine catalyst;

the tertiary amine catalyst accounts for 3-7% of the total mass of the coagulating bath.

Has the advantages that: book (I)The invention provides a soft, light, thin and super-warm aerogel filling material for shoes, clothes, bedding and mattress, which is prepared by compounding profiled fibers and round fibers and adding polyether polyurethane dispersoid containing epoxy groups and SiO₂The dispersion compounded by aerogel, tertiary amine catalyst, sodium polyacrylate and maleic acid-acrylic acid copolymer adopts a dipping-foaming process, and solves the problems that the conventional synthetic chemical fiber has poor dimensional stability, is easy to deform after being washed by water for many times and has SiO₂The problem that the aerogel is easy to fall off and lose the heat retention property, and the problem that foaming raw materials are not uniformly distributed in the water foaming process and foaming speed is too high in the preparation process of the filling material, so that foam holes are not uniform, the stability and uniformity in the foaming process are improved, the prepared filling material not only has good air permeability and moisture conductivity, but also has good dimensional stability and heat retention property after being washed for multiple times, and the requirements of people on soft, light, thin, air permeable and super-heat-retention clothes are met.

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 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.

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.

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 method for manufacturing a soft, light, thin and super-thermal aerogel filling material for shoes, clothes, bedding and the like, which comprises the following steps:

In the present invention, the nonwoven fabric may be prepared by using a machine cloth method well known to those skilled in the art.

In some embodiments, the raw material of the glue solution at least comprises SiO₂Aerogel, polyurethane binder, organic solvent.

In the present invention, the glue solution can be prepared by using a dispersing mode, SiO, which is well known to those skilled in the art₂The aerogel is insoluble in organic solvent, and is dispersed in the organic solvent in the form of powder or particles, the macromolecular chains of the polyurethane adhesive are arranged in a random coil shape, and then the organic solvent of the micromolecules is slowly changed along with the macromolecular chains of the polyurethane adhesiveThe polyurethane adhesive moves and continuously permeates into macromolecular chains to weaken the cohesion of the macromolecular chains, so that the loosening and stretching of the coil macromolecular chains are accelerated, namely the polyurethane adhesive is dissolved in an organic solvent.

In the present invention, the impregnation of the nonwoven fabric may be performed by a known impregnation method, i.e., the nonwoven fabric is put into a glue solution, the glue solution is infiltrated into the nonwoven fabric, and the obtained nonwoven fabric has SiO₂Aerogel and organic solvent with dissolved polyurethane binder.

In the invention, the water foaming is to introduce the non-woven fabric into a coagulating bath for coagulation foaming, then introduce the non-woven fabric into a washing tank for washing so as to clean the residual organic solvent on the non-woven fabric, then introduce the washed non-woven fabric into a dryer for drying and reinforcing, and finally modify the non-woven fabric to obtain the filling material.

In some embodiments, the coagulation bath comprises water, a catalyst;

the temperature of the coagulation bath is 33-35 ℃;

the water washing temperature is 75-85 ℃;

the drying temperature is 90-105 ℃.

In the invention, the specific principle of the water foaming is as follows: the organic solvent of embedding in the non-woven fabrics is run out from between polyurethane macromolecule chain by water replacement, accompanies the entering of hydrone simultaneously, and polyurethane is insoluble in water for the looks cohesion between macromolecule chain increases, and along with organic solvent's continuous reduction and polyurethane macromolecule chain looks polymerization form irregular clew and arrange, polyurethane constantly contracts and solidifies, and then the production bubble. The whole foaming process involves two processes, namely the external diffusion of an organic solvent and the internal diffusion of water, the relative speeds of the two determine the foaming speed, at the initial stage of foaming, the concentration difference of the internal and external organic solvents is large, the outward diffusion speed of the organic solvent is high, if water molecules cannot be rapidly diffused inwards, the outward diffusion speed of the organic solvent is far greater than the inward diffusion speed of the water molecules, the surface which is firstly contacted with water is rapidly solidified into a film, and then the inward diffusion of the water molecules is blocked, so that the bubbles on the surface of the non-woven fabric are large and large, the bubbles inside the non-woven fabric are small or uneven, and the prepared filling material is hard, and the air permeability and the moisture conductivity are poor.

The invention provides a soft, light and thin super-thermal aerogel filling material for the bedding and the shoes, and the filling material is prepared by processing non-woven fabrics and glue solution;

the raw material of the glue solution comprises SiO₂Aerogel, organic solvent.

< nonwoven Fabric >

The non-woven fabric is a fabric formed by weaving fabric without yarn, and is formed by forming a fiber web structure by orienting or randomly arranging the short fiber or filament and then reinforcing the fiber web structure by adopting a mechanical method, a thermal bonding method or a chemical method.

In some embodiments, the raw material of the nonwoven fabric is selected from the group consisting of shaped fibers, round fibers.

(Special-shaped fiber)

The profiled fiber is made by a spinneret with non-circular holes in the spinning forming process and has various cross-sectional shapes.

In some embodiments, the shaped fiber is selected from the group consisting of triangular shaped fiber, Y shaped fiber, pentagonal shaped fiber, trilobal shaped fiber, quadrilobal shaped fiber, pentalobal shaped fiber, fan shaped fiber, hollow shaped fiber.

In a preferred embodiment, the shaped fiber is a triangular shaped fiber.

In a more preferred embodiment, the mass ratio of the triangular profiled fibers to the round fibers is (1-4): 8.

in a further preferred embodiment, the triangular shaped fibers and the round fibers have a mass ratio of 1: 4.

the triangular profiled fiber is not particularly limited, and can be various triangular profiled fibers conventionally used by those skilled in the art, and can be obtained commercially, for example, the commercially available triangular profiled fiber includes but is not limited to the product (polyester filament fiber) with the product number of 22, which is purchased from Jinxia, Zhejiang, New materials and technology Co., Ltd.

The round fibers are not particularly limited in the present invention, and may be various round fibers conventionally used by those skilled in the art, and may be commercially available, for example, commercially available round fibers including, but not limited to, products (polyester filament fibers) available from salicornia armata chemical fiber ltd.

<SiO₂Aerogel>

Aerogel, also called xerogel, is solid in appearance and is the solid with the lowest density in the world when most of the solvent is removed from the gel, so that the liquid content in the gel is much less than the solid content, or the medium filled in the space network structure of the gel is gas. There are many kinds of aerogels including silicon-based, carbon-based, sulfur-based, metal oxide-based, metal-based, etc., among which silicon-based is SiO₂An aerogel.

In some embodiments, the aerogel is SiO₂An aerogel.

In a preferred embodiment, the SiO is₂The aperture of the aerogel is 20-30 nm.

The SiO of the invention₂Aerogels, commercially available, e.g. commercially available SiO₂The aerogel includes but is not limited to products (product form: granule, powder; color: white, blue; bulk density: 40-150 kg/m) purchased from QIAGEN technologies of Jiangxi Bo³(ii) a Specific surface area: 500 to 1000; porosity:>90 percent; pore diameter: 10 to 30 nm).

< organic solvent >

The organic solvent is an organic compound which is liquid at normal temperature and normal pressure, can dissolve some organic compounds which are insoluble in water, has higher volatility, and has no change in the properties of a solute and the solvent in the dissolving process.

In some embodiments, the organic solvent is selected from the group consisting of dimethylformamide, acetone, butanone, toluene, xylene, ethyl acetate, propylene glycol butyl ether, propylene glycol methyl ether acetate.

In a preferred embodiment, the organic solvent is dimethylformamide.

(dimethylformamide)

Dimethylformamide, dmf (dimethyl formamide) for short, CAS number 68-12-2, is a transparent liquid, is a polar organic solvent with high boiling point, can be mutually soluble with water and most organic solvents, can be used as a solvent for polyurethane, polyacrylonitrile and polyvinyl chloride, and also can be used as a raw material for an extracting agent, medicines and pesticide imidacloprid.

The inventor finds that the non-woven fabric prepared by compounding the triangular profiled fibers and the round fibers can maintain better dimensional stability after being soaked and foamed and the prepared filling material is washed for multiple times. The inventors speculate that the possible reasons are: the triangular profiled fibers have irregular cross sections and are mutually staggered with the round fibers, so that the friction force among the fibers is increased, the anti-sliding capacity among the fibers is improved, and the size of the filling material is stable.

The inventor also finds that compared with the filling material prepared from single profiled fiber or single round fiber, the filling material prepared by compounding triangular profiled fiber and round fiber has better air permeability and moisture permeability. The inventors speculate that the possible reasons are as follows:

firstly, the triangular profiled fibers have irregular cross section shapes, and gaps between fiber surfaces generated by the unique cross section shapes substantially improve the air permeability and moisture permeability of the filling material; secondly, the triangular special-shaped fiber and the round fiber are compounded, the deformation possibility of the special-shaped fiber is reduced, the unique section shape of the special-shaped fiber is well maintained, and the air permeability and the moisture retention of the filling material are ensured. However, the profiled fibers are expensive, so that the mixing amount of the profiled fibers is not too large, and experiments prove that when the mass ratio of the profiled fibers to the round fibers is (1-4): and 8, the prepared filling material is light, thin, breathable and warm-keeping.

In addition, in combination with the above foaming principle, the possible reasons are technically presumed to be: firstly, in the process of impregnating the non-woven fabric with the glue solution, the gaps among the fibers are beneficial to the glue solution to uniformly penetrate into the non-woven fabric, namely, SiO is ensured₂Aerogel and polyurethane are uniformly distributed inside and outside the non-woven fabric; secondly, in the water foaming process, the gaps between the surfaces of the fibers are beneficial to quickly and uniformly distributing water inside and outside the non-woven fabric, the foaming speed is controlled, and the prepared filling material has uniform foam pores.

In some embodiments, the glue solution further comprises a binder.

In some embodiments, the raw material of the glue solution further comprises a dispersant.

In some embodiments, the coagulation bath further comprises a catalyst.

< adhesive agent >

In some embodiments, the adhesive is selected from a polyether polyurethane adhesive, a polyester polyurethane adhesive. The polyether/polyester polyurethane adhesive is a polymer obtained by polymerizing a polyvalent isocyanate compound and a polyether/polyester containing active hydrogen atoms.

In a preferred embodiment, the binder is an epoxy-containing polyether polyurethane dispersion.

In a more preferred embodiment, the particle size of the epoxy group-containing polyether polyurethane dispersion is 50 to 100 nm.

(epoxy-containing polyether urethane dispersion)

The preparation method of the epoxy group-containing polyether polyurethane dispersion with the particle size of 50-100 nm comprises the following steps:

adding epoxy propanol and polyoxypropylene glycol into a 1000ml three-necked bottle, heating to 100-110 ℃, carrying out vacuum dehydration for 2 hours until the water content is lower than 0.05%, then adding 2, 4-toluene diisocyanate, carrying out rapid stirring, carrying out a reaction at 70-80 ℃, cooling to room temperature after the prepolymerization reaction is finished, diluting with a solvent, then dropwise adding a 1, 4-butanediol chain extender at room temperature for chain extension, and after the reaction is carried out for a period of time, placing into a 50 ℃ water bath, and carrying out a reaction for 1 hour to obtain a polyether polyurethane dispersion with relatively stable properties and containing an epoxy group;

diluting the prepared polyether polyurethane dispersion containing the epoxy groups by 200 times with deionized water, and testing with a zeta potential nanometer particle size analyzer to obtain the polyether polyurethane dispersion with the particle size uniformly distributed in the range of 50-100 nm.

The polyoxypropylene diol of the present invention is not particularly limited, and may be any of various polyoxypropylene diols conventionally used by those skilled in the art, and may be commercially available, for example, commercially available polyoxypropylene diols including, but not limited to, products (content ≧ 99.99%) available from Jining HuaKai resin Co., Ltd.

< catalyst >

The catalyst of the invention is placed in a coagulation bath.

In some embodiments, the catalyst is selected from amine catalysts, metal alkyl catalysts.

In a preferred embodiment, the catalyst is a tertiary amine catalyst;

As examples of the tertiary amine catalyst, there may be mentioned: triethylenediamine, N-alkylmorpholine, bis (2-methyloxyethyl) ether, triethylamine, dimethylbenzylamine.

In a more preferred embodiment, the tertiary amine catalyst is triethylenediamine.

(triethylenediamine)

Triethylenediamine (TEDA) with CAS number of 280-57-9, which is colorless or white crystal in normal state, is easy to absorb moisture and agglomerate when exposed to air, is alkaline, and can absorb CO in air₂Yellowing, solubility in acetone, benzene and ethanol, and solubility in straight-chain hydrocarbon solvents such as pentane.

The inventors have found that the thermal insulation properties of the filling material are more durable when using the epoxy-containing polyether polyurethane dispersion as a binder. The inventors speculate that possible causes are: first, SiO₂A large number of hydroxyl groups are distributed on the surface of the aerogel and can react with residual-NCO groups in the polyurethane adhesive to generate firm chemical bonds such as urethane bonds or urea bonds, so that firm bonding is realized; secondly, in the invention, the non-woven fabric prepared by compounding the triangular profiled fibers and the round fibers is used as the base fabric, and the profiled fibers have irregular cross sections, more irregular gaps are formed by interlacing the fibers, and the non-woven fabric is provided with SiO₂The adhesive molecules of the aerogel penetrate into the gaps of the base cloth to form stronger mechanical engagement force, thereby enhancing the SiO₂Adhesion between aerogel and non-woven fabric.

Meanwhile, the inventor finds that when the particle size of the epoxy group-containing polyether polyurethane dispersion is 50-100 nm, the prepared filling material has good heat retention property, and has excellent air permeability and moisture retention property. The inventors speculate that possible causes are: firstly, the viscosity of the glue solution is influenced by the particle size of the polyurethane dispersoid, when the particle size is 50-100 nm, the viscosity of the glue solution is moderate, the problem that the glue solution cannot uniformly penetrate into the non-woven fabric due to overlarge viscosity is solved, the problem that the glue solution cannot uniformly penetrate into the non-woven fabric due to too small viscosity and poor bonding property between the glue solution and the non-woven fabric is solved, and finally the glue solution uniformly penetrates into the inside and the outside of the non₂Aerogel and polyurethane are uniformly distributed inside and outside the non-woven fabric; next, SiO in the present invention₂The pore diameter of the aerogel is 20-30 nm, and polyurethane dispersoid with the particle diameter of 50-100 nm cannot enter pores of the aerogel, so that the aerogel is prevented from losing the capacity of the porous material for storing air, insulating heat and preserving heat.

The present inventors have also surprisingly found that the temperature during the consolidation of the nonwoven fabric can be reduced from 200 ℃ to 90 ℃ without destroying the cross-sectional shape of the profiled fibers and without affecting the performance of the binder. The inventors speculate that possible causes are: at the temperature of more than 90 ℃, the epoxy group of the polyether polyurethane adhesive containing the epoxy group is opened under the action of the catalyst and reacts with the hydrolyzed hydroxyl or carboxyl of the polyurethane adhesive, so that the crosslinking degree of the adhesive is improved, and the adhesive property of the adhesive is ensured.

< dispersant >

The dispersant is used for uniformly dispersing inorganic and organic solid and liquid particles which are difficult to dissolve in liquid, and simultaneously preventing the particles from settling and coagulating.

In some embodiments, the dispersant is selected from the group consisting of sodium polyacrylate, sodium polymetaphosphate, sodium orthophosphate, sodium pyrophosphate, sodium linoleate, sodium citrate, potassium citrate, sodium silicate, maleic-acrylic acid copolymer, carboxymethyl cellulose.

(Polysodium acrylate)

Sodium polyacrylate, PAAS (polymeric Acid sodium) for short in English, CAS number 9003-04-7, is a novel functional polymer material and an important chemical product, the solid product is white (or light yellow) block or powder, the liquid product is colorless (or light yellow) viscous liquid, is dissolved in media such as cold water, warm water, glycerol, propylene glycol and the like, is stable to temperature change, and has the effect of fixing metal ions.

(maleic acid-acrylic acid copolymer)

Maleic acid-acrylic acid copolymer, abbreviated as MA/AA (copolymer of Maleic and acrylic acid) in English, has CAS number of 26677-99-6, is a low molecular weight polyelectrolyte, is prepared by copolymerizing Maleic acid and acrylic acid according to a certain proportion, has high thermal stability and strong chelating force to metal ions, and can also be used as a chelating dispersant.

In a preferred embodiment, the dispersant is a combination of sodium polyacrylate and maleic acid-acrylic acid copolymer.

In a preferred embodiment, the mass of the maleic-acrylic acid copolymer in the formulation is not less than 5% of the mass of the sodium polyacrylate.

The sodium polyacrylate of the present invention is not particularly limited, and may be various sodium polyacrylates conventionally used by those skilled in the art, and may be commercially available, for example, commercially available sodium polyacrylate includes, but is not limited to, a product (specific gravity: 1.15; melting point: 12.5 ℃ C.; boiling point: 141 ℃ C.) of model M29077 available from Michelle chemical technology Co., Ltd., Shanghai.

The maleic acid-acrylic acid copolymer of the present invention is not particularly limited, and may be various maleic acid-acrylic acid copolymers conventionally used by those skilled in the art, and may be commercially available, for example, commercially available maleic acid-acrylic acid copolymers include, but are not limited to, products available from chemistry of Guangdong, Wengjiang, Inc., model number PB 98792.

The inventor finds that the heat retention of the filling material can be improved by adding the sodium polyacrylate into the glue solution, and the heat retention of the filling material is further improved by adding the sodium polyacrylate and the maleic acid-acrylic acid copolymer. The inventors speculate that possible causes are: firstly, sodium polyacrylate plays the role of a dispersing agent in glue solution, so that SiO can be enabled₂Uniformly dispersing aerogel in the glue solution; and secondly, the sodium polyacrylate can be precipitated with metal ions in water in the water foaming process to reduce the dispersion effect of the sodium polyacrylate, and the maleic acid-acrylic acid copolymer has a stronger adsorption effect on the metal ions, does not generate precipitates and plays a role in protecting the sodium polyacrylate. Experiments prove that when the mass of the maleic acid-acrylic acid copolymer in the compound is not less than 5% of the mass of the sodium polyacrylate, the maleic acid-acrylic acid copolymer can fully adsorb metal ions in water, and the dispersion effect of the sodium polyacrylate is ensured.

Meanwhile, the inventor unexpectedly finds that when the compound of sodium polyacrylate and maleic acid-acrylic acid copolymer is added as the dispersing agent, foam holes generated in the foaming process are more uniform, so that the prepared filling material has better air permeability and moisture permeability. The inventors speculate that possible causes are: firstly, sodium polyacrylate is embedded into the non-woven fabric, external water can quickly enter the non-woven fabric in the water foaming process, the relative speed of the external diffusion of the organic solvent and the internal diffusion of the water is reduced, and the foaming speed is further controlled, so that the foam holes formed inside and outside the non-woven fabric are more uniform and stable, namely the foaming speed is controlled from the diffusion angle; secondly, the maleic acid-acrylic acid copolymer and the catalyst in the coagulating bath act synergistically to delay the occurrence of polyurethane coagulation shrinkage in the foaming process, so that water molecules have sufficient time to uniformly diffuse into the non-woven fabric without obstruction, and the uniform internal foaming is ensured, namely the foaming speed is controlled from the point of delaying the occurrence of coagulation. But in order to prevent the coagulation from being delayed, the sodium polyacrylate in the coagulating bath has more consumption with water, so that the dispersing effect of the sodium polyacrylate is poor, and experiments prove that when the catalyst accounts for 3-7% of the total mass of the coagulating bath, the dispersing effect and the relatively delayed coagulation are ensured.

Examples

Example 1

Embodiment 1 provides a soft, light and thin super thermal aerogel filling material for shoes, clothes, bedding and the like, wherein the filling material is manufactured by processing non-woven fabrics and glue solution.

The raw materials of the non-woven fabric comprise profiled fibers and round fibers which are respectively purchased from Zhejiang Jinxia New Material science and technology company and sea salt Tianma chemical fiber company;

the mass ratio of the profiled fibers to the round fibers is 1: 8.

the glue solution comprises the following raw materials in parts by weight: SiO 2₂4 parts of aerogel, 50 parts of adhesive, 4.2 parts of dispersing agent (4 parts of sodium polyacrylate and 0.2 part of maleic acid-acrylic acid copolymer) and 200 parts of organic solvent.

The SiO₂The aerogel has a pore size of 20 to 30nm and is available from QIAGEN technologies of Jiangxi Bo.

The adhesive is polyether polyurethane dispersion containing epoxy groups, and the preparation method comprises the following steps:

adding 20 parts of epoxy propanol and 20 parts of polyoxypropylene glycol into a 1000ml three-necked bottle according to parts by weight, heating to 100 ℃, carrying out vacuum dehydration for 2 hours until the water content is lower than 0.05%, then adding 80 parts of 2, 4-toluene diisocyanate, rapidly stirring, reacting at 80 ℃, cooling to room temperature after the prepolymerization reaction is finished, diluting with acetone, then dropwise adding 40 parts of 1, 4-butanediol chain extender at room temperature for chain extension, and after reacting for a period of time, placing into a 50 ℃ water bath, and continuously reacting for 1 hour to obtain the epoxy group-containing polyether polyurethane dispersion with relatively stable property;

diluting the prepared polyether polyurethane dispersion containing the epoxy group by 200 times with deionized water, and testing with a zeta potential nanometer particle size analyzer to obtain a dispersion with an average particle size of 80 nm;

the polyoxypropylene diol was purchased from Jining HuaKai resin Co., Ltd.

The dispersing agent is a compound of sodium polyacrylate and maleic acid-acrylic acid copolymer;

the sodium polyacrylate is purchased from Shanghai Michelle chemical technology Co., Ltd, and has the model number of M29077;

the maleic acid-acrylic acid copolymer was purchased from Guangdong Wengjiang chemical reagent, Inc. and was designated as PB 98792.

The organic solvent is dimethylformamide.

The mass fraction of the catalyst in the coagulation bath was 3%.

The catalyst is triethylenediamine.

The manufacturing method of the soft, light, thin and super-thermal aerogel filling material for the shoes, the clothes and the bedding comprises the following steps:

s1, preparing non-woven fabrics from the profiled fibers and the round fibers according to the mass ratio in a machine cloth mode;

s2, mixing SiO₂Dispersing a complex of aerogel, polyether polyurethane dispersion containing epoxy groups, sodium polyacrylate and maleic acid-acrylic acid copolymer in dimethyl formamide according to parts by weight to obtain a glue solution;

s4, carrying SiO in S3₂Placing the non-woven fabric of the aerogel into a coagulating bath at the temperature of 35 ℃ for coagulating foaming, then placing into a water washing tank at the temperature of 80 ℃ for water washing to wash residual organic solvent, then introducing the non-woven fabric after water washing into a dryer for drying and reinforcing at the temperature of 100 ℃, and finally performing correction treatment to obtain the filling material.

Example 2

Embodiment 2 provides a soft, light and thin super-thermal aerogel filling material for shoes, clothes, bedding and the like, wherein the filling material is manufactured by processing non-woven fabrics, glue solution and coagulating bath.

the mass ratio of the profiled fibers to the round fibers is 1: 2.

the glue solution comprises the following raw materials in parts by weight: SiO 2₂8 parts of aerogel, 70 parts of adhesive, 21.2 parts of dispersing agent (20 parts of sodium polyacrylate and 1.2 parts of maleic acid-acrylic acid copolymer) and 300 parts of organic solvent.

The adhesive was an epoxy-containing polyether polyurethane dispersion prepared as in example 1.

The organic solvent is dimethylformamide.

The mass fraction of the catalyst in the coagulation bath was 7%.

The catalyst is triethylenediamine.

The manufacturing method of the soft, light, thin and super-thermal aerogel filling material for the shoes, the clothes, the bedding and the like is the same as that in the embodiment 1.

Example 3

Embodiment 3 provides a soft, light and thin super-thermal aerogel filling material for shoes, clothes, bedding and the like, wherein the filling material is manufactured by processing non-woven fabrics, glue solution and coagulating bath.

the mass ratio of the profiled fibers to the round fibers is 1: 4.

the glue solution comprises the following raw materials by weightThe components in parts by weight: SiO 2₂6 parts of aerogel, 60 parts of adhesive, 12.6 parts of dispersing agent (12 parts of sodium polyacrylate and 0.6 part of maleic acid-acrylic acid copolymer) and 250 parts of organic solvent.

The organic solvent is dimethylformamide.

The mass fraction of the catalyst in the coagulation bath is 5%.

The catalyst is triethylenediamine.

Comparative example 1

Comparative example 1 compared with example 3, the non-woven fabric has no foreign fiber, the raw material of the non-woven fabric is round fiber, and the rest is the same as example 3.

Comparative example 2

Comparative example 2 compared with example 3, the round fiber was not included, the nonwoven fabric was made of triangular profiled fiber, and the rest was the same as example 3.

Comparative example 3

Comparative example 3 compared to example 3, the mass ratio of triangular profiled fibers to round fibers was 0.1: the rest was the same as in example 3.

Comparative example 4

Comparative example 4 compared to example 3, the mass ratio of triangular profiled fibers to round fibers was 2: 1, the other points are the same as in example 3.

Comparative example 5

Comparative example 5 in comparison to example 3, the binder was a polyester polyurethane dispersion prepared by the steps of:

adding 30 parts of polyethylene glycol adipate into a 1000ml three-necked bottle according to the parts by weight, heating to 100 ℃, carrying out vacuum dehydration for 2 hours until the water content is lower than 0.05%, then adding 80 parts of 2, 4-toluene diisocyanate, carrying out rapid stirring, reacting at 80 ℃, cooling to room temperature after the prepolymerization reaction is finished, diluting with acetone, then dropwise adding 35 parts of 1, 4-butanediol chain extender at room temperature for chain extension, and after reacting for a period of time, placing into a 50 ℃ water bath for continuous reaction for 1 hour to obtain the polyester polyurethane with relatively stable property.

The rest is the same as in example 3.

Comparative example 6

Comparative example 6 has no catalyst as compared with example 3, and the rest is the same as example 3.

Comparative example 7

Comparative example 7 compared to example 3, the catalyst was benzyltriethylammonium chloride, otherwise the same as in example 3.

Comparative example 8

Comparative example 8 compared to example 3, there was no sodium polyacrylate, otherwise the same as example 3.

Comparative example 9

Comparative example 9 compared to example 3, there was no maleic acid-acrylic acid copolymer, otherwise the same as example 3.

Comparative example 10

Comparative example 10 compared to example 3, there was no sodium polyacrylate and maleic acid-acrylic acid copolymer, otherwise the same as example 3.

Comparative example 11

Comparative example 11 the mass fraction of the catalyst in the coagulation bath was 0.5% as compared with example 3, and the rest was the same as example 3.

Comparative example 12

Comparative example 12 the mass fraction of the catalyst in the coagulation bath was 20% as compared with example 3, and the rest was the same as example 3.

Evaluation of Performance

1. Test of Heat Retention Performance

The test is carried out according to GB/T11048-.

2. Test for air permeability

The test was carried out according to GB/T5453-1997 determination of the air permeability of textile fabrics, the test results being expressed in terms of air permeability.

3. Moisture permeability test

The test is carried out according to GB/T12704-.

4. Dimensional stability test

The filling materials obtained in examples 1 to comparative example 12 were washed 5 times and 10 times, respectively, with reference to ISO 6330-2000 household washing and drying procedure for textile testing.

The shrinkage of the filling material after washing is determined with reference to ISO 3759-2007 preparation, marking and measurement of garment and fabric samples for textile determination dimensional change test.

5. Test of warming property after washing

The test is carried out according to GB/T11048 + 2008' determination of thermal resistance and wet resistance of textile under the steady-state condition of physiological comfort.

Table 1 performance characterization test

As can be seen from examples 1-3 in Table 1, the soft, light and thin super-thermal aerogel filling material for the bedding and the shoes in the invention has good heat preservation, air permeability and moisture conductivity, and can maintain good size and thermal insulation performance after being washed for many times.

The preparation method of the embodiment of the disclosure only relates to the compounds related to the embodiment of the disclosure, and other compounds can refer to the general preparation method.

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

1. A soft, light and thin super-thermal aerogel filling material for shoes, clothes, bedding and is characterized in that the filling material is manufactured by processing non-woven fabrics and glue solution;

the raw materials of the non-woven fabric are triangular profiled fibers and round fibers;

the mass ratio of the triangular profiled fibers to the round fibers is (1-4): 8;

the raw material of the glue solution comprises SiO₂Aerogels, organic solvents, binders;

the adhesive is an epoxy-containing polyether polyurethane dispersion;

2. The soft, thin and ultra-warm aerogel packing material for footwear, clothing, bedding and the like according to claim 1, wherein the SiO is₂The aperture of the aerogel is 20-30 nm.

3. The soft, light, thin and ultra-warm aerogel filling material for the shoes, clothes, bedding and the like as claimed in claim 1, wherein the raw material of the glue solution further comprises a dispersing agent.

4. The soft, light, thin and ultra-warm aerogel filling material for the footwear, clothing, bedding and the like according to claim 3, wherein the dispersing agent is a compound of sodium polyacrylate and maleic acid-acrylic acid copolymer.

5. The soft, light, thin and ultra-warm aerogel filling material for the footwear, clothing, bedding and the like according to claim 4, wherein the mass of the maleic acid-acrylic acid copolymer in the compound is not less than 5% of the mass of the sodium polyacrylate.

6. A method for manufacturing soft, thin and ultra-warm aerogel packing material for footwear, clothing, bedding and other articles according to any of claims 1-5, comprising the steps of:

s1, preparing the non-woven fabric by the triangular profiled fibers and the round fibers in a non-woven fabric manufacturing mode through a machine;

s2, mixing SiO in the raw material of the glue solution₂Dispersing aerogel and adhesive in an organic solvent to obtain a glue solution;

7. The method for manufacturing soft, lightweight, thin, ultra-thermal aerogel packing material for footwear, clothing, bedding, and other articles of claim 6 wherein the coagulation bath further comprises a catalyst;

the catalyst is tertiary amine catalyst;