CN114957783B - Inorganic fiber composite foam material and preparation method thereof - Google Patents

Inorganic fiber composite foam material and preparation method thereof Download PDF

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CN114957783B
CN114957783B CN202210600122.9A CN202210600122A CN114957783B CN 114957783 B CN114957783 B CN 114957783B CN 202210600122 A CN202210600122 A CN 202210600122A CN 114957783 B CN114957783 B CN 114957783B
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fiber
foam material
basalt fiber
composite foam
basalt
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CN114957783A (en
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宋顺喜
赵俊帆
任玮
张美云
谭蕉君
戢德贤
黎凌浩
王倩玉
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Shaanxi University of Science and Technology
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/30—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof by mixing gases into liquid compositions or plastisols, e.g. frothing with air
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/0014—Use of organic additives
    • C08J9/0023—Use of organic additives containing oxygen
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/0014—Use of organic additives
    • C08J9/0033—Use of organic additives containing sulfur
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/009—Use of pretreated compounding ingredients
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2329/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal, or ketal radical; Hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Derivatives of such polymer
    • C08J2329/02—Homopolymers or copolymers of unsaturated alcohols
    • C08J2329/04—Polyvinyl alcohol; Partially hydrolysed homopolymers or copolymers of esters of unsaturated alcohols with saturated carboxylic acids

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Abstract

The application discloses an inorganic fiber composite foam material and a preparation method thereof, belongs to the technical field of inorganic fiber composite materials and sound-absorbing and heat-insulating materials, and solves the technical problems that the existing inorganic and fiber-based sound-absorbing and heat-insulating composite materials are difficult to form, high in brittleness, poor in compressibility, low in sound absorption in broadband, high in weight, poor in heat preservation and heat insulation, inflammable and the like. The application discloses a preparation method of an inorganic fiber composite foam material, which adopts basalt fibers as a framework, and converts an open-cell material into an adjustable semi-open-cell material by inducing the polyvinyl alcohol fibers to generate morphological change in the preparation process of the composite foam through temperature, so as to solve the problems of difficult molding, large brittleness, poor compressibility, health risk, wide frequency low sound absorption, large weight, poor heat preservation and insulation, flammability and the like of the existing inorganic and fiber-based sound-absorbing and heat-insulating materials; the preparation process is simple and feasible, is environment-friendly and easy to expand, and expands the application of the high-performance basalt fiber in the fields of sound absorption, heat insulation and structural weight reduction.

Description

Inorganic fiber composite foam material and preparation method thereof
Technical Field
The application belongs to the technical field of inorganic fiber composite materials and sound-absorbing and heat-insulating materials, and particularly relates to an inorganic fiber composite foam material and a preparation method thereof.
Background
Fiber-based porous foam materials have been under great attention in academia and industry due to their excellent properties of low cost, light weight, high porosity, etc., and have been widely studied. Most of the porous materials have interconnected regular or irregular open-cell, semi-closed-cell and closed-cell structures, so that the porous materials have wide application potential in the fields of heat preservation, heat insulation, sound absorption, noise reduction, drug delivery, packaging, oil-water separation and the like. Among them, inorganic fiber foam materials are receiving more and more attention in the fields of sound absorption, noise reduction, heat preservation and heat insulation because of their excellent strength and temperature resistance, and the advantages of small heat conductivity, fire resistance, moisture resistance, corrosion resistance, low price, etc. The traditional inorganic sound-absorbing and heat-insulating ceramic fiber and asbestos fiber show good performances of high and low temperature resistance, sound absorption and noise reduction and the like due to viscous loss and heat conversion of sound and heat energy in the pores inside the fiber-based open-pore material, but the materials have the defects of difficult molding, high brittleness, poor compressibility, wide frequency, low sound absorption, high density, poor heat preservation and heat insulation, flammability and the like, and the use requirements of the high-performance sound-absorbing and heat-insulating product are difficult to meet.
Basalt fiber is an excellent inorganic fiber material, and the main component is SiO 2 And Al 2 O 3 The material has outstanding high modulus, high strength, good temperature resistance, excellent chemical stability, sound absorption performance and electrical insulation performance, so that the material is used as a 'twenty-first-year green industrial material' with low cost and high performance and is used as a sound absorption flame retardant material. However, basalt is smooth in surface, poor in hydrophilicity and easy to cause polarization of water molecules due to the existence of liquid surface tension in the production process of basalt, so that the surface of the basalt is negatively charged, static electricity is generated between fibers, the fibers are intertwined and are difficult to disperse, poor binding force with a matrix interface is caused, and further application of the basalt in multiple fields is limited.
Disclosure of Invention
In order to overcome the defects of the prior art, the application aims to provide an inorganic fiber composite foam material and a preparation method thereof, which are used for solving the technical problems of difficult molding, large brittleness, poor compressibility, health risk, wide frequency band, low sound absorption, large weight, poor heat preservation and insulation, flammability and the like of the traditional inorganic fiber-based sound-absorbing and heat-insulating composite material.
In order to achieve the above purpose, the application is realized by adopting the following technical scheme:
the application discloses a preparation method of an inorganic fiber composite foam material, which comprises the following steps:
s1: carrying out heat treatment on the basalt fiber to obtain a basalt fiber after heat treatment; mixing the basalt fiber after heat treatment, concentrated sulfuric acid and hydrogen peroxide, and obtaining basalt fiber after acid treatment; washing and drying the basalt fiber subjected to acid treatment to obtain modified basalt fiber;
s2: carrying out fluffing dispersion treatment, suction filtration and dehydration on the modified basalt fiber to obtain basalt fiber slurry; mixing basalt fiber sizing agent and polyvinyl alcohol fiber, and foaming to obtain mixed sizing agent A; mixing the mixed slurry A and a decahydrate sodium tetraborate solution to obtain a mixed solution, regulating the pH value of the mixed solution, and stirring to obtain a mixed slurry B;
s3: mixing the mixed slurry B with a surfactant, and bubbling to obtain foam slurry C; foaming the foam slurry C to obtain a foam material preform D; and drying the foam material preform D to obtain the inorganic fiber composite foam material.
Further, in S1, the heat treatment mode is calcination, the calcination temperature is 300-400 ℃, and the calcination time is 1-3 hours; the washing is carried out by adopting deionized water until the washing liquid obtained by washing is neutral; the drying is carried out in an oven, the temperature of the drying is 85-125 ℃, and the time of the drying is 0.5-3 h.
Further, in S1, the dosage ratio of the basalt fiber to the concentrated sulfuric acid to the hydrogen peroxide is (1-50 g) g: (7-210) mL: (3-90) mL; the temperature of the mixing treatment is 60-95 ℃; the concentration of the concentrated sulfuric acid is 1-4 mol/L.
Further, in S2, the fluffing and dispersing treatment is carried out by adopting a fluffer, wherein the dispersing concentration of the modified basalt fiber in the fluffer is 0.1-0.2 wt% and the dispersing time is 1-5min; the concentration of basalt fiber in the basalt fiber slurry is 5-15 wt%.
Further, in S2, the mass ratio of the basalt fiber slurry to the polyvinyl alcohol fiber is (50-95): (5-50); the polyvinyl alcohol fiber is a hot melt fiber, the diameter is 20 mu m, the length is 4mm, and the melting point is 60-90 ℃; the pH of the mixed solution was adjusted to 10.
Further, in S2, the stirring is mechanical stirring, the rotating speed of the mechanical stirring is 1000-4000 rpm, and the time of the mechanical stirring is 10-60min; the ratio of the absolute dry mass of the fiber in the mixed slurry A to the dosage of the sodium tetraborate decahydrate solution is 5g: (0.22-2.60 g); the pH value of the mixed solution is regulated by adopting one of NaOH solution, KOH solution or Ca (OH) 2 solution, and the concentration of the NaOH solution, the KOH solution or the Ca (OH) 2 solution is 1-6 mol/L.
Further, in S3, the surfactant is one or two of sodium dodecyl sulfate and polyvinyl alcohol, and the mass fraction of the surfactant is 2-10wt%; the dosage ratio of the mixed slurry B to the surfactant is 1L: (0.2-0.6 g).
Further, in S3, the bubbling adopts a mechanical bubbling mode, and the rotating speed of the mechanical bubbling is 2000-4000 rpm; the foaming time is 5-30 min.
Further, in S3, the drying is performed at 60-120 ℃ for 1-3 hours.
The application also discloses the inorganic fiber composite foam material prepared by the preparation method, and the density of the inorganic fiber composite foam material is 8-12mg/cm 3 。
Compared with the prior art, the application has the following beneficial effects:
the application discloses a preparation method of an inorganic fiber composite foam material, which adopts basalt fibers as a framework, and converts an open-cell material into an adjustable semi-open-cell material by inducing the polyvinyl alcohol fibers to generate morphological change in the preparation process of the composite foam through temperature, so as to solve the application problems of difficult molding, large brittleness, poor compressibility, health risk, wide frequency, low sound absorption, large weight, poor heat preservation and insulation, flammability and the like of the traditional inorganic and fiber-based sound-absorption and heat-insulation composite material; the preparation method is simple, has low cost and has great application potential in commercial houses and industrial buildings. In addition, the preparation method of the application provides a simple and effective fiber-membrane structure, the morphology of the polyvinyl alcohol fibers is changed, so that the original contact mode between fibers is converted into the mode between fibers and between the fibers, the bonding sites between the fibers are increased, the contact area is increased, when the gravity load is increased, the stress is converted into the plastic deformation of the fiber-membrane structure from the limited deformation between the original fibers, the compression strength of the material is increased, and a feasible new idea is provided for overcoming the brittleness of the material and enhancing the compression strength of the inorganic fiber material. In addition, the preparation method provided by the application can realize structure regulation and control only under a lower temperature condition, is simple in preparation process, pollution-free in process and low in energy consumption, and is an effective, environment-friendly and easy to expand method.
Further, the application adopts the surfactant to mix sodium dodecyl sulfate with polyvinyl alcohol and mixed slurry B, the hot-melt polyvinyl alcohol fiber is transformed into a film-shaped substance from the fiber form through temperature induction, the fibers are transformed into fiber coating and adhesion from original intertwining, so as to form a fiber-film structure, the compression performance of the material is improved, meanwhile, the structure is transformed into a semi-closed pore material from fiber open pores, the propagation tortuous path of sound energy and heat energy in the semi-closed pore material is increased, the sound energy and heat energy dissipation is increased, the sound absorption and heat insulation performance is further improved, a novel method for transforming the foam material into the semi-open pore and closed pore material from open pores is provided, and a novel scheme is provided for the commercial sound absorption and heat insulation material.
The application also discloses the inorganic fiber composite foam material prepared by the preparation method, and the inorganic fiber composite foam material has ultralow density of 8-12mg/cm 3 The super-light material range is reached, the super-light material has great potential in the fields of commercial sound-absorbing heat-insulating material weight reduction and structural material weight reduction, advances the development of basalt fiber products, expands the application of high-performance basalt fibers in the fields of sound-absorbing heat insulation and structural weight reduction, and ensures that the inorganic fiber foam has broad prospects in the application fields of sound-absorbing heat insulation and the like.
Drawings
FIG. 1 is a scanning electron microscope image of an inorganic fiber composite foam material prepared in example 5 of the present application;
FIG. 2 is a schematic compression diagram of an inorganic fiber composite foam material prepared in example 5 of the present application;
wherein: a-polyvinyl alcohol fibers; b. c and d-images of different magnifications of the inorganic fiber composite foam;
FIG. 3 is a graph showing the sound absorption of the inorganic fiber composite foam material prepared in example 5 of the present application;
FIG. 4 is a thermal insulation image of the inorganic fiber composite foam material prepared in example 5 of the present application;
Detailed Description
So that those skilled in the art can appreciate the features and effects of the present application, a general description and definition of the terms and expressions set forth in the specification and claims follows. Unless otherwise defined, 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 application belongs, and in the event of a conflict, the present specification shall control.
The theory or mechanism described and disclosed herein, whether right or wrong, is not meant to limit the scope of the application in any way, i.e., the present disclosure may be practiced without limitation to any particular theory or mechanism.
All features such as values, amounts, and concentrations that are defined herein in the numerical or percent ranges are for brevity and convenience only. Accordingly, the description of a numerical range or percentage range should be considered to cover and specifically disclose all possible sub-ranges and individual values (including integers and fractions) within the range.
Herein, unless otherwise indicated, "comprising," "including," "having," or similar terms encompass the meanings of "consisting of … …" and "consisting essentially of … …," e.g., "a includes a" encompasses the meanings of "a includes a and the other and" a includes a only.
In this context, not all possible combinations of the individual technical features in the individual embodiments or examples are described in order to simplify the description. Accordingly, as long as there is no contradiction between the combinations of these technical features, any combination of the technical features in the respective embodiments or examples is possible, and all possible combinations should be considered as being within the scope of the present specification.
The application will be further illustrated with reference to specific examples. It is to be understood that these examples are illustrative of the present application and are not intended to limit the scope of the present application. Furthermore, it should be understood that various changes and modifications can be made by one skilled in the art after reading the teachings of the present application, and such equivalents are intended to fall within the scope of the application as defined in the appended claims.
The following examples use instrumentation conventional in the art. The experimental methods, in which specific conditions are not noted in the following examples, are generally conducted under conventional conditions or under conditions recommended by the manufacturer. The following examples used various starting materials, unless otherwise indicated, were conventional commercial products, the specifications of which are conventional in the art. In the description of the present application and the following examples, "%" means weight percent, and "parts" means parts by weight, and ratios means weight ratio, unless otherwise specified.
The preparation method of the inorganic fiber composite foam material specifically comprises the following steps:
(1) Inorganic fiber modification: calcining basalt fibers in a muffle furnace at 300-400 ℃ for 1-3h to obtain pretreated basalt fibers; placing the pretreated basalt fiber into a mixed solution of concentrated sulfuric acid and hydrogen peroxide for treatment for 1h, wherein the volume ratio of the concentrated sulfuric acid to the hydrogen peroxide is 7:3, the treatment temperature is 60-95 ℃ to obtain basalt fiber treated by acid; continuously washing the basalt fiber subjected to acid treatment by deionized water until the pH test paper is neutral, and drying the basalt fiber in an oven at 85-125 ℃ for 0.5-3 h to obtain the dried modified basalt fiber.
(2) Inorganic fiber slurry preparation: dispersing the basalt fiber prepared in the step 1 in a fluffer, wherein the dispersion concentration of the basalt fiber in the fluffer is 0.1-0.2 wt%The dispersing time is 1-5 min. And (3) carrying out suction filtration and dehydration on the basalt fiber dispersion liquid to obtain basalt fiber with the concentration of 5-15 wt%, wherein the basalt fiber has the diameter of 11-16 mu m and the length of 4-8 mm. And placing the basalt fiber slurry and polyvinyl alcohol fibers in a foaming container to prepare mixed slurry A. Wherein, the mass ratio of basalt fiber to polyvinyl alcohol fiber is (50-95): (50-5), wherein the polyvinyl alcohol fiber has a diameter of 20 μm and a length of 4mm. To the mixed slurry a, a prepared sodium tetraborate decahydrate solution was added, wherein the ratio of the absolute dry mass of the fibers in the mixed slurry a to the amount of the sodium tetraborate decahydrate solution was 5g: (0.22-2.60 g), adjusting pH to 10, and mechanically stirring to obtain uniformly mixed slurry B, wherein the pH adjusting solvent is NaOH, KOH and Ca (OH) 2 One of them has the concentration of 1 mol/L-6 mol/L, the mechanical stirring rotation speed of 1000-4000 rpm and the stirring and mixing time of 20-60min.
(3) Preparation of inorganic fiber foam material: and (2) adding a surfactant into the mixed slurry B obtained in the step (2), and mechanically stirring to obtain uniform foam slurry C, wherein the surfactant is one or two of sodium dodecyl sulfate and polyvinyl alcohol solution, the mass fraction of the surfactant is 5wt%, the adding amount of the surfactant is 0.2-1.2 g/L, the mechanical bubbling rotating speed is 2000-4000 rpm, and the foaming time is 5-30 min. And after foaming is completed, transferring the foam slurry into a forming device for water filtering to obtain a foam material preform D.
(4) And (5) drying and forming: transferring the foam material preform D obtained in the step (3) into a blast drying oven, and drying at the temperature of 60-120 ℃ for 1-3h to obtain the inorganic fiber composite foam material.
According to the inorganic fiber composite foam material and the preparation method thereof disclosed by the application, basalt fibers are taken as a framework, and the polyvinyl alcohol fibers are induced to generate morphological changes in the preparation process of the composite foam through temperature, so that an open-cell material is converted into an adjustable semi-open-cell material, and the problems of difficult molding, high brittleness, poor compressibility, health risks, wide frequency low sound absorption, heavy weight, poor heat preservation and insulation, flammability and the like of the conventional inorganic fiber-based sound-absorption and heat-insulation composite material are solved. The application designs a quick and effective fiber-membrane structure by adopting a novel method, and the open-pore-closed pore ratio is regulated by temperature, so that the optimal air flow resistance is generated, the bending and internal reflection of sound wave propagation are increased, the basalt fiber-based composite foam which is adjustable in open-pore-closed pore ratio, low in density, enhanced in sound absorption and noise reduction, excellent in compression rebound, low in heat conductivity and self-extinguishing is produced, and the technical blank of the current high-performance basalt fiber composite material is filled.
Example 1
A method for preparing an inorganic fiber composite foam material, which comprises the following steps:
step 1: modification of inorganic fibers: calcining 3.75g basalt fiber in a muffle furnace at 300 ℃ for 1h to obtain heat-treated basalt fiber; placing the basalt fiber after heat treatment in a mixed solution of concentrated sulfuric acid and hydrogen peroxide for treatment for 1h, wherein the volume ratio of the concentrated sulfuric acid to the hydrogen peroxide is 7:3, processing at 60 ℃ to obtain basalt fibers subjected to acid treatment; continuously washing the basalt fiber subjected to acid treatment by deionized water until the pH test paper is neutral, and drying the basalt fiber in an oven at 105 ℃ for 3 hours to obtain a dried modified basalt fiber with the diameter of 12 mu m and the length of 4mm;
step 2: dispersing the modified basalt fiber obtained in the step 1 in a fluffer, wherein the dispersion concentration of the modified basalt fiber in the fluffer is 0.1wt%, the fluffing and dispersing time is 3min, so as to obtain a dispersion liquid, and filtering and dehydrating the dispersion liquid to obtain basalt fiber slurry with the concentration of 5%; placing basalt fiber sizing agent and polyvinyl alcohol fiber into a foaming container for mixing, and foaming to obtain mixed sizing agent A; wherein the mass ratio of basalt fiber slurry to polyvinyl alcohol fiber is 75:25, the diameter of the polyvinyl alcohol fiber is 20 mu m, and the length is 4mm; then adding 0.22g of sodium tetraborate decahydrate solution into the mixed slurry A to obtain a mixed solution, regulating the pH value of the mixed solution to 10 by adopting 2mol/L KOH solution, and stirring and crosslinking at a rotating speed of 1000rpm for 20min to obtain mixed slurry B;
step 3: mixing the mixed slurry B obtained in the step 2 with 5wt% of sodium dodecyl sulfate, wherein the adding amount of the sodium dodecyl sulfate is 0.2g/L; a uniformly foamed composite fiber foam precursor C is obtained by a mechanical bubbling mode, after the foaming time is 20min, the foam slurry is transferred to a forming device for water filtering, and a foam material preform D is obtained; and transferring the foam material preform D into a blast drying oven, and drying at 100 ℃ for 2 hours to obtain the inorganic fiber composite foam material.
Example 2
A method for preparing an inorganic fiber composite foam material, which comprises the following steps:
step 1: modification of inorganic fibers: calcining 4g basalt fiber in a muffle furnace at 300 ℃ for 2 hours to obtain basalt fiber after heat treatment; placing the basalt fiber after heat treatment in a mixed solution of concentrated sulfuric acid and hydrogen peroxide for treatment for 1h, wherein the volume ratio of the concentrated sulfuric acid to the hydrogen peroxide is 7:3, the treatment temperature is 70 ℃, and basalt fibers treated by acid are obtained; continuously washing the basalt fiber subjected to acid treatment by deionized water until the pH test paper is neutral, and drying the basalt fiber in an oven at 85 ℃ for 2 hours to obtain a dried modified basalt fiber with the diameter of 11 mu m and the length of 6 mm;
step 2: dispersing the modified basalt fiber obtained in the step 1 in a fluffer, wherein the dispersion concentration of the modified basalt fiber in the fluffer is 0.2wt%, the fluffing and dispersing time is 5min, so as to obtain a dispersion liquid, and filtering and dehydrating the dispersion liquid to obtain basalt fiber slurry with the concentration of 10%; placing basalt fiber sizing agent and polyvinyl alcohol fiber into a foaming container for mixing, and foaming to obtain mixed sizing agent A; wherein the mass ratio of basalt fiber slurry to polyvinyl alcohol fiber is 80:20, the diameter of the polyvinyl alcohol fiber is 20 mu m, and the length is 4mm; then adding 1.73g of sodium tetraborate decahydrate solution into the mixed slurry A to obtain a mixed solution, regulating the pH value of the mixed solution to 10 by adopting a KOH solution with the concentration of 4mol/L, and stirring and crosslinking at the rotation speed of 1000rpm for 20min to obtain mixed slurry B;
step 3: mixing the mixed slurry B obtained in the step 2 with 5wt% of sodium dodecyl sulfate, wherein the adding amount of the sodium dodecyl sulfate is 0.2g/L; a uniformly foamed composite fiber foam precursor C is obtained by a mechanical bubbling mode, after the foaming time is 20min, the foam slurry is transferred to a forming device for water filtering, and a foam material preform D is obtained; and transferring the foam material preform D into a blast drying oven, and drying at 100 ℃ for 2 hours to obtain the inorganic fiber composite foam material.
Example 3
A method for preparing an inorganic fiber composite foam material, which comprises the following steps:
step 1: modification of inorganic fibers: calcining 4g basalt fiber in a muffle furnace at 400 ℃ for 1h to obtain basalt fiber after heat treatment; placing the basalt fiber after heat treatment in a mixed solution of concentrated sulfuric acid and hydrogen peroxide for treatment for 1h, wherein the volume ratio of the concentrated sulfuric acid to the hydrogen peroxide is 7:3, processing at 60 ℃ to obtain basalt fibers subjected to acid treatment; continuously washing the basalt fiber subjected to acid treatment by deionized water until the pH test paper is neutral, and drying in an oven at 125 ℃ for 1h to obtain a dried modified basalt fiber with the diameter of 16 mu m and the length of 8 mm;
step 2: dispersing the modified basalt fiber obtained in the step 1 in a fluffer, wherein the dispersion concentration of the modified basalt fiber in the fluffer is 0.1wt%, the fluffing and dispersing time is 1min, so as to obtain a dispersion liquid, and filtering and dehydrating the dispersion liquid to obtain basalt fiber slurry with the concentration of 10%; placing basalt fiber sizing agent and polyvinyl alcohol fiber into a foaming container for mixing, and foaming to obtain mixed sizing agent A; wherein the mass ratio of basalt fiber slurry to polyvinyl alcohol fiber is 80:20, the diameter of the polyvinyl alcohol fiber is 20 mu m, and the length is 4mm; then adding 0.87g of 4wt% sodium tetraborate decahydrate solution into the mixed slurry A to obtain a mixed solution, regulating the pH value of the mixed solution to be 10 by adopting 2mol/L NaOH solution, and stirring and crosslinking at 2000rpm for 20min to obtain mixed slurry B;
step 3: mixing the mixed slurry B obtained in the step 2 with a polyvinyl alcohol solution with the mass fraction of 5wt%, wherein the addition amount of the polyvinyl alcohol solution is 0.6g/L; a uniformly foamed composite fiber foam precursor C is obtained by a mechanical bubbling mode, after the foaming time is 5min, the foam slurry is transferred to a forming device for water filtering, and a foam material preform D is obtained; and transferring the foam material preform D into a blast drying oven, and drying at 120 ℃ for 2 hours to obtain the inorganic fiber composite foam material.
Example 4
A method for preparing an inorganic fiber composite foam material, which comprises the following steps:
step 1: modification of inorganic fibers: calcining 4.75g basalt fiber in a muffle furnace at 350 ℃ for 2 hours to obtain heat-treated basalt fiber; placing the basalt fiber after heat treatment in a mixed solution of concentrated sulfuric acid and hydrogen peroxide for treatment for 1h, wherein the volume ratio of the concentrated sulfuric acid to the hydrogen peroxide is 7:3, processing at 95 ℃ to obtain basalt fibers subjected to acid treatment; continuously washing the basalt fiber subjected to acid treatment by deionized water until the pH test paper is neutral, and drying the basalt fiber in an oven at 105 ℃ for 1h to obtain dried modified basalt fiber with the diameter of 14 mu m and the length of 8 mm;
step 2: dispersing the modified basalt fiber obtained in the step 1 in a fluffer, wherein the dispersion concentration of the modified basalt fiber in the fluffer is 0.15wt%, the fluffing and dispersing time is 5min, so as to obtain a dispersion liquid, and filtering and dehydrating the dispersion liquid to obtain basalt fiber slurry with the concentration of 10%; placing basalt fiber sizing agent and polyvinyl alcohol fiber into a foaming container for mixing, and foaming to obtain mixed sizing agent A; wherein the mass ratio of basalt fiber slurry to polyvinyl alcohol fiber is 95:5, the diameter of the polyvinyl alcohol fiber is 20 mu m, and the length is 4mm; subsequently, 2.60g of a sodium tetraborate decahydrate solution was added to the mixed slurry A to obtain a mixed solution, and 2mol/L of Ca (OH) was used 2 The pH value of the mixed solution is regulated to 10, and then the mixed solution is stirred and crosslinked for 60 minutes at a rotating speed of 3000rpm to obtain mixed slurry B;
step 3: mixing the mixed slurry B obtained in the step 2 with a polyvinyl alcohol solution with the mass fraction of 5wt%, wherein the addition amount of the polyvinyl alcohol solution is 0.6g/L; a uniformly foamed composite fiber foam precursor C is obtained by a mechanical bubbling mode, after the foaming time is 5min, the foam slurry is transferred to a forming device for water filtering, and a foam material preform D is obtained; and transferring the foam material preform D into a blast drying oven, and drying at the temperature of 60 ℃ for 2 hours to obtain the inorganic fiber composite foam material.
Example 5
A method for preparing an inorganic fiber composite foam material, which comprises the following steps:
step 1: modification of inorganic fibers: calcining 3.5g basalt fiber in a muffle furnace at 350 ℃ for 2 hours to obtain basalt fiber after heat treatment; placing the basalt fiber after heat treatment in a mixed solution of concentrated sulfuric acid and hydrogen peroxide for treatment for 1h, wherein the volume ratio of the concentrated sulfuric acid to the hydrogen peroxide is 7:3, the treatment temperature is 90 ℃, and basalt fibers treated by acid are obtained; continuously washing the basalt fiber subjected to acid treatment by deionized water until the pH test paper is neutral, and drying the basalt fiber in an oven at 105 ℃ for 2 hours to obtain a dried modified basalt fiber with the diameter of 15 mu m and the length of 4mm;
step 2: dispersing the modified basalt fiber obtained in the step 1 in a fluffer, wherein the dispersion concentration of the modified basalt fiber in the fluffer is 0.2wt%, the fluffing and dispersing time is 5min, so as to obtain a dispersion liquid, and filtering and dehydrating the dispersion liquid to obtain basalt fiber slurry with the concentration of 10%; placing basalt fiber sizing agent and polyvinyl alcohol fiber into a foaming container for mixing, and foaming to obtain mixed sizing agent A; wherein the mass ratio of basalt fiber slurry to polyvinyl alcohol fiber is 70:30, the diameter of the polyvinyl alcohol fiber is 20 mu m, and the length is 4mm; then adding 1.73g of 1wt% sodium tetraborate decahydrate solution into the mixed slurry A to obtain a mixed solution, regulating the pH value of the mixed solution to be 10 by adopting 4mol/L NaOH solution, and stirring and crosslinking at 2000rpm for 60min to obtain mixed slurry B;
step 3: mixing the mixed slurry B obtained in the step 2 with a polyvinyl alcohol solution with the mass fraction of 5wt%, wherein the addition amount of the polyvinyl alcohol solution is 0.6g/L; a uniformly foamed composite fiber foam precursor C is obtained by a mechanical bubbling mode, after the foaming time is 5min, the foam slurry is transferred to a forming device for water filtering, and a foam material preform D is obtained; and transferring the foam material preform D into a blast drying oven, and drying at the temperature of 95 ℃ for 2 hours to obtain the inorganic fiber composite foam material.
Example 6
A method for preparing an inorganic fiber composite foam material, which comprises the following steps:
step 1: modification of inorganic fibers: 2.5g basalt fiber is placed in a muffle furnace at 350 ℃ for calcination, and the calcination time is 3 hours, so that basalt fiber after heat treatment is obtained; placing the basalt fiber after heat treatment in a mixed solution of concentrated sulfuric acid and hydrogen peroxide for treatment for 1h, wherein the volume ratio of the concentrated sulfuric acid to the hydrogen peroxide is 7:3, processing at 60 ℃ to obtain basalt fibers subjected to acid treatment; continuously washing the basalt fiber subjected to acid treatment by deionized water until the pH test paper is neutral, and drying the basalt fiber in an oven at 90 ℃ for 0.5h to obtain a dried modified basalt fiber with the diameter of 13 mu m and the length of 6 mm;
step 2: dispersing the modified basalt fiber obtained in the step 1 in a fluffer, wherein the dispersion concentration of the modified basalt fiber in the fluffer is 0.2wt%, the fluffing and dispersing time is 5min, so as to obtain a dispersion liquid, and filtering and dehydrating the dispersion liquid to obtain basalt fiber slurry with the concentration of 10%; placing basalt fiber sizing agent and polyvinyl alcohol fiber into a foaming container for mixing, and foaming to obtain mixed sizing agent A; wherein the mass ratio of basalt fiber slurry to polyvinyl alcohol fiber is 50:50, the diameter of the polyvinyl alcohol fiber is 20 mu m, and the length is 4mm; then adding 1.73g of sodium tetraborate decahydrate solution into the mixed slurry A to obtain a mixed solution, regulating the pH value of the mixed solution to 10 by adopting 6mol/L NaOH solution, and stirring and crosslinking at 4000rpm for 60min to obtain mixed slurry B;
step 3: mixing the mixed slurry B obtained in the step 2 with a polyvinyl alcohol solution with the mass fraction of 5wt%, wherein the adding amount of the polyvinyl alcohol solution is 0.2g/L; a uniformly foamed composite fiber foam precursor C is obtained by a mechanical bubbling mode, after the foaming time is 5min, the foam slurry is transferred to a forming device for water filtering, and a foam material preform D is obtained; and transferring the foam material preform D into a blast drying oven, and drying at 100 ℃ for 2 hours to obtain the inorganic fiber composite foam material.
Example 7
A method for preparing an inorganic fiber composite foam material, which comprises the following steps:
step 1: modification of inorganic fibers: calcining 4.25g basalt fiber in a muffle furnace at 350 ℃ for 3 hours to obtain basalt fiber after heat treatment; placing the basalt fiber after heat treatment in a mixed solution of concentrated sulfuric acid and hydrogen peroxide for treatment for 1h, wherein the volume ratio of the concentrated sulfuric acid to the hydrogen peroxide is 7:3, the treatment temperature is 35 ℃, and basalt fibers treated by acid are obtained; continuously washing the basalt fiber subjected to acid treatment by deionized water until the pH test paper is neutral, and drying the basalt fiber in an oven at 120 ℃ for 3 hours to obtain a dried modified basalt fiber with the diameter of 14 mu m and the length of 4mm;
step 2: dispersing the modified basalt fiber obtained in the step 1 in a fluffer, wherein the dispersion concentration of the modified basalt fiber in the fluffer is 0.2wt%, the fluffing and dispersing time is 5min, so as to obtain a dispersion liquid, and filtering and dehydrating the dispersion liquid to obtain basalt fiber slurry with the concentration of 10%; placing basalt fiber sizing agent and polyvinyl alcohol fiber into a foaming container for mixing, and foaming to obtain mixed sizing agent A; wherein the mass ratio of basalt fiber slurry to polyvinyl alcohol fiber is 85:15, the diameter of the polyvinyl alcohol fiber is 20 mu m, and the length is 4mm; then adding 2.60g of sodium tetraborate decahydrate solution into the mixed slurry A to obtain a mixed solution, regulating the pH value of the mixed solution to be 10 by adopting a KOH solution with the concentration of 1mol/L, and stirring and crosslinking at the rotation speed of 1000rpm for 10min to obtain mixed slurry B;
step 3: mixing the mixed slurry B obtained in the step 2, and 5wt% of polyvinyl alcohol solution and sodium dodecyl sulfate, wherein the addition amount of the polyvinyl alcohol solution and the sodium dodecyl sulfate is 0.2g/L; a uniformly foamed composite fiber foam precursor C is obtained by a mechanical bubbling mode, after the foaming time is 30min, the foam slurry is transferred to a forming device for water filtering, and a foam material preform D is obtained; and transferring the foam material preform D into a blast drying oven, and drying at 65 ℃ for 2 hours to obtain the inorganic fiber composite foam material.
Example 8
A method for preparing an inorganic fiber composite foam material, which comprises the following steps:
step 1: modification of inorganic fibers: placing 5g basalt fiber in a muffle furnace at 400 ℃ for calcination for 0.5h to obtain basalt fiber after heat treatment; placing the basalt fiber after heat treatment in a mixed solution of concentrated sulfuric acid and hydrogen peroxide for treatment for 1h, wherein the volume ratio of the concentrated sulfuric acid to the hydrogen peroxide is 21:9, obtaining basalt fiber treated by acid, wherein the treatment temperature is 60 ℃; continuously washing the basalt fiber subjected to acid treatment by deionized water until the pH test paper is neutral, and drying the basalt fiber in an oven at 85 ℃ for 0.5h to obtain a dried modified basalt fiber with the diameter of 14 mu m and the length of 4mm;
step 2: dispersing the modified basalt fiber obtained in the step 1 in a fluffer, wherein the dispersion concentration of the modified basalt fiber in the fluffer is 0.2wt%, the fluffing and dispersing time is 5min, so as to obtain a dispersion liquid, and filtering and dehydrating the dispersion liquid to obtain basalt fiber slurry with the concentration of 15%; placing basalt fiber sizing agent and polyvinyl alcohol fiber into a foaming container for mixing, and foaming to obtain mixed sizing agent A; wherein the mass ratio of basalt fiber slurry to polyvinyl alcohol fiber is 85:15, the diameter of the polyvinyl alcohol fiber is 20 mu m, and the length is 4mm; then adding 2.30g of sodium tetraborate decahydrate solution into the mixed slurry A to obtain a mixed solution, regulating the pH value of the mixed solution to 10 by adopting 5mol/L KOH solution, and stirring and crosslinking at 4000rpm for 10min to obtain mixed slurry B;
step 3: mixing the mixed slurry B obtained in the step 2, and 10wt% of polyvinyl alcohol solution and sodium dodecyl sulfate, wherein the addition amount of the polyvinyl alcohol solution and the sodium dodecyl sulfate is 0.2g/L; a uniformly foamed composite fiber foam precursor C is obtained by a mechanical bubbling mode, after the foaming time is 5min, the foam slurry is transferred to a forming device for water filtering, and a foam material preform D is obtained; and transferring the foam material preform D into a blast drying oven, and drying at the temperature of 60 ℃ for 2 hours to obtain the inorganic fiber composite foam material.
The basalt fiber/polyvinyl alcohol fiber composite foam prepared in the embodiment 5 of the application has the performance characterization, and the density is 9mg/cm 3 As can be seen from the compression test image of fig. 2, the foam still recovers its original shape when the foam compression set reaches 80%. As shown in FIG. 1, the apparent appearance of the prepared composite foam is observed, and as shown in FIG. 1a, the polyvinyl alcohol fiber with the diameter of 20 mu m and the length of 4mm used in the application is changed in shape in the composite foam under the induction of the forming temperature of 95 ℃, and is converted into a film shape from fiber shape to film shape to be adhered and coated on adjacent basalt fibers, so that a part of fiber-film structure is formed, and the proportion of the closed pore shape of the foam material is increased. As shown in FIG. 3, the sound absorption test was conducted by cutting the sample into cylinders with diameters of 3cm and 10cm by using a transfer function method and referring to GB/T18696.2-2002 and ISO 10534-2:2001 to measure sound absorption coefficients of sound absorption characteristics in the frequency ranges of 63-1600Hz and 1000-6300z, respectively, and the obtained material was increased in absorption coefficient with the increase of frequency, and had excellent sound absorption coefficient at middle and high frequencies, and the sound absorption performance of the material was evaluated by Noise Reduction Coefficient (NRC), which is an average value of sound absorption coefficients of 250, 500, 1000 and 2000Hz, and the foam NRC obtained in example 5 was 0.4, and had light weight and excellent sound absorption performance. As shown in fig. 4, which shows the thermal insulation performance characterization of the material, the composite foam was placed on a bottom heating table at 150 ℃ to observe the trend of the temperature of the top of the foam over time, the top of the foam was 34.0 ℃ when the composite foam was placed for 10min, the top temperature was 39.5 ℃ and the top temperature was 47.0 ℃ when the composite foam was placed for 20min, the difference between the top temperature and the platform temperature was 103 ℃, and the composite foam exhibited excellent thermal insulation performance.
The above is only for illustrating the technical idea of the present application, and the protection scope of the present application is not limited by this, and any modification made on the basis of the technical scheme according to the technical idea of the present application falls within the protection scope of the claims of the present application.

Claims (9)

1. A method for preparing an inorganic fiber composite foam material, which is characterized by comprising the following steps:
s1: carrying out heat treatment on the basalt fiber to obtain a basalt fiber after heat treatment; mixing the basalt fiber after heat treatment, concentrated sulfuric acid and hydrogen peroxide, and obtaining basalt fiber after acid treatment; washing and drying the basalt fiber subjected to acid treatment to obtain modified basalt fiber;
s2: carrying out fluffing dispersion treatment, suction filtration and dehydration on the modified basalt fiber to obtain basalt fiber slurry; mixing basalt fiber sizing agent and polyvinyl alcohol fiber, and foaming to obtain mixed sizing agent A; mixing the mixed slurry A and a decahydrate sodium tetraborate solution to obtain a mixed solution, regulating the pH value of the mixed solution, and stirring to obtain a mixed slurry B; the polyvinyl alcohol fibers are hot melt fibers, the diameter is 20 mu m, the length is 4mm, and the melting point is 60-90 ℃;
s3: mixing the mixed slurry B with a surfactant, and bubbling to obtain foam slurry C; foaming the foam slurry C to obtain a foam material preform D; drying the foam material preform D to obtain an inorganic fiber composite foam material; and the drying is carried out at 60-120 ℃ for 1-3 hours.
2. The method for preparing the inorganic fiber composite foam material according to claim 1, wherein in the step S1, the heat treatment mode is calcination, the calcination temperature is 300-400 ℃, and the calcination time is 1-3 hours; the washing is carried out by adopting deionized water until the washing liquid obtained by washing is neutral; the drying is carried out in an oven, the temperature of the drying is 85-125 ℃, and the time of the drying is 0.5-3 h.
3. The method for preparing the inorganic fiber composite foam material according to claim 1, wherein in S1, the dosage ratio of the basalt fiber, the concentrated sulfuric acid and the hydrogen peroxide is (1-50) g: (7-210) mL: (3-90) mL; the temperature of the mixing treatment is 60-95 ℃; the concentration of the concentrated sulfuric acid is 1-4 mol/L.
4. The preparation method of the inorganic fiber composite foam material according to claim 1, wherein in the step S2, the fluffing and dispersing treatment is carried out by adopting a fluffer, the dispersing concentration of the modified basalt fiber in the fluffer is 0.1-0.2wt%, and the dispersing time is 1-5min; the concentration of basalt fibers in the basalt fiber slurry is 5-15 wt%.
5. The preparation method of the inorganic fiber composite foam material according to claim 1, wherein in S2, the mass ratio of the basalt fiber slurry to the polyvinyl alcohol fiber is (50-95): (5-50); the pH of the mixed solution was adjusted to 10.
6. The method for preparing the inorganic fiber composite foam material according to claim 1, wherein in the step S2, the stirring is mechanical stirring, the rotating speed of the mechanical stirring is 1000-4000 rpm, and the time of the mechanical stirring is 10-60min; the ratio of the absolute dry mass of the fiber in the mixed slurry A to the dosage of the sodium tetraborate decahydrate solution is 5g: (0.22-2.60 g); the pH value of the mixed solution is regulated by adopting NaOH solution, KOH solution or Ca (OH) 2 One of the solutions is regulated, either NaOH solution, KOH solution or Ca (OH) 2 The concentration of the solution is 1-6 mol/L.
7. The preparation method of the inorganic fiber composite foam material according to claim 1, wherein in S3, the surfactant is one or two of sodium dodecyl sulfate and polyvinyl alcohol, and the mass fraction of the surfactant is 2-10wt%; the dosage ratio of the mixed slurry B to the surfactant is 1L: (0.2 to 0.6) g.
8. The method for preparing the inorganic fiber composite foam material according to claim 1, wherein in the step S3, the bubbling adopts a mechanical bubbling mode, and the mechanical bubbling speed is 2000-4000 rpm; the foaming time is 5-30 min.
9. By using the method of claim 1 to 8The inorganic fiber composite foam material prepared by the preparation method of any one of the inorganic fiber composite foam materials is characterized in that the density of the inorganic fiber composite foam material is 8-12mg/cm 3 。
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