CN113858739A - Reinforced fiber polymer composite wallboard with natural network framework and preparation method - Google Patents

Reinforced fiber polymer composite wallboard with natural network framework and preparation method Download PDF

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CN113858739A
CN113858739A CN202111098700.5A CN202111098700A CN113858739A CN 113858739 A CN113858739 A CN 113858739A CN 202111098700 A CN202111098700 A CN 202111098700A CN 113858739 A CN113858739 A CN 113858739A
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composite material
layer
parts
loofah sponge
natural
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CN113858739B (en
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郭勇
汪浩
陈玉霞
刘光辉
徐润民
张清扬
周娟
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Anhui Agricultural University AHAU
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/34—Layered products comprising a layer of synthetic resin comprising polyamides
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/12—Layered products comprising a layer of synthetic resin next to a fibrous or filamentary layer
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    • B32B33/00—Layered products characterised by particular properties or particular surface features, e.g. particular surface coatings; Layered products designed for particular purposes not covered by another single class
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    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
    • B32B37/06—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the heating method
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
    • B32B37/10—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the pressing technique, e.g. using action of vacuum or fluid pressure
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B5/00—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts
    • B32B5/02—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by structural features of a fibrous or filamentary layer
    • B32B5/028—Net structure, e.g. spaced apart filaments bonded at the crossing points
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L77/00—Compositions of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Compositions of derivatives of such polymers
    • C08L77/02—Polyamides derived from omega-amino carboxylic acids or from lactams thereof
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L99/00—Compositions of natural macromolecular compounds or of derivatives thereof not provided for in groups C08L89/00 - C08L97/00
    • E—FIXED CONSTRUCTIONS
    • E04—BUILDING
    • E04F—FINISHING WORK ON BUILDINGS, e.g. STAIRS, FLOORS
    • E04F13/00—Coverings or linings, e.g. for walls or ceilings
    • E04F13/07—Coverings or linings, e.g. for walls or ceilings composed of covering or lining elements; Sub-structures therefor; Fastening means therefor
    • E04F13/08—Coverings or linings, e.g. for walls or ceilings composed of covering or lining elements; Sub-structures therefor; Fastening means therefor composed of a plurality of similar covering or lining elements
    • E04F13/0875—Coverings or linings, e.g. for walls or ceilings composed of covering or lining elements; Sub-structures therefor; Fastening means therefor composed of a plurality of similar covering or lining elements having a basic insulating layer and at least one covering layer
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2262/00—Composition or structural features of fibres which form a fibrous or filamentary layer or are present as additives
    • B32B2262/06—Vegetal fibres
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/10—Properties of the layers or laminate having particular acoustical properties
    • B32B2307/102—Insulating
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/50—Properties of the layers or laminate having particular mechanical properties
    • B32B2307/558—Impact strength, toughness
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    • B32—LAYERED PRODUCTS
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    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/70—Other properties
    • B32B2307/732—Dimensional properties
    • B32B2307/734—Dimensional stability
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2607/00—Walls, panels
    • B32B2607/02—Wall papers, wall coverings
    • E—FIXED CONSTRUCTIONS
    • E04—BUILDING
    • E04F—FINISHING WORK ON BUILDINGS, e.g. STAIRS, FLOORS
    • E04F2290/00—Specially adapted covering, lining or flooring elements not otherwise provided for
    • E04F2290/04—Specially adapted covering, lining or flooring elements not otherwise provided for for insulation or surface protection, e.g. against noise, impact or fire
    • E04F2290/041—Specially adapted covering, lining or flooring elements not otherwise provided for for insulation or surface protection, e.g. against noise, impact or fire against noise

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Abstract

The invention provides a reinforced fiber polymer composite wallboard with a natural network framework, which comprises a composite material film layer and a loofah sponge network structure layer; the composite material film layer is provided with a plurality of layers, and each layer comprises the following raw materials in parts by weight: 50-60 parts of PA 6-citric acid blend, 40-50 parts of pine nut powder, 2-3 parts of a dispersing agent and 1-3 parts of a coupling agent; the loofah sponge network structure layer is embedded between the composite material thin layers, and each layer comprises the following raw materials in parts by weight: 4-8 parts of loofah sponge network fiber and 1-6 parts of an adhesive. The invention also provides a preparation method of the reinforced fiber polymer composite wallboard with the natural network framework. The invention has the advantages that: the preparation method can avoid the problems of weak compatibility and poor mechanical property of a composite interface caused by adopting the traditional plant fiber/plastic composite material, and also has the advantages of wide raw material source, low cost and environmental protection.

Description

Reinforced fiber polymer composite wallboard with natural network framework and preparation method
Technical Field
The invention relates to the technical field of fiber polymer composite materials, in particular to a reinforced fiber polymer composite wallboard with a natural network framework and a preparation method thereof.
Background
The plant fiber is a composite material of the filler. Through the rapid development of the past decades, the plant fiber/plastic composite material with good performance has been widely applied to the fields of building, decoration, furniture manufacturing and transportation, and the like, and the commercialization process of the plant fiber/plastic composite material also effectively reduces the environmental pollution and the resource waste. However, in the plant fiber/plastic composite material, the polarity of the fiber is opposite to that of the plastic, so that the interface compatibility of the composite material is weak, and the mechanical property of the material is poor. This problem limits to some extent the utilization of natural fibres as renewable resources.
The loofah sponge fiber is a porous plant fiber material which can be directly obtained from nature and can be repeatedly obtained, has the characteristics of rich resources, wide sources, reproducibility, degradability, environmental protection and no toxicity, and also has the natural structural characteristics of low density, high porosity, specific strength, high specific modulus, large amount of hydroxyl functional groups on the surface and the like. Meanwhile, the loofah sponge fiber has a three-dimensional reticular hollow structure formed by criss-cross three-dimensional reticular fibers, and the structural characteristics can effectively improve the mechanical property and the dimensional stability of the material.
Polyamide 6(PA6), known as polycaprolactam, commonly known as nylon 6, is a translucent or opaque, milky-white, semi-crystalline thermoplastic polymer made mainly of omega-aminocaproic acid or caprolactam by polymerization, with caprolactam as the starting material being more commonly produced. The PA6 has a regular molecular chain structure and a strong polar amide group, so that the PA6 has good comprehensive performance, including good crystallinity, mechanical strength (tensile strength can reach 50-60 MPa, and bending strength can reach 80-90 MPa), heat resistance, low friction coefficient, chemical resistance and self-lubricity, is easy to process and form, and has a large applicable temperature range.
Therefore, if the loofah sponge fiber and the polyamide 6 are mixed and combined with a certain amount of dispersing agent, adhesive, coupling agent and the like to prepare the reinforced fiber polymer composite material with the natural network framework, the problem of poor mechanical property of the existing plant fiber/plastic composite material can be effectively solved, and the material has the advantages of wide raw material source, low cost, environmental friendliness and the like.
Disclosure of Invention
The invention aims to solve the technical problem of providing a reinforced fiber polymer composite wallboard with a natural network framework and a preparation method thereof, which can avoid the problems of weak composite interface compatibility and poor mechanical property caused by adopting the traditional plant fiber/plastic composite material, and simultaneously has the advantages of wide raw material source, low cost and environmental protection.
The invention adopts the following technical scheme to solve the technical problems:
a reinforced fiber polymer composite wallboard with natural network skeleton comprises a composite material film layer and a loofah sponge network structure layer; the composite material film layer is provided with a plurality of layers, and each layer comprises the following raw materials in parts by weight: 50-60 parts of PA 6-citric acid blend, 40-50 parts of pine nut powder, 2-3 parts of a dispersing agent and 1-3 parts of a coupling agent; the loofah sponge network structure layer is embedded between the composite material thin layers, and each layer comprises the following raw materials in parts by weight: 4-8 parts of loofah sponge network fiber and 1-6 parts of an adhesive.
As one of the preferable modes of the invention, the composite material film layer is provided with 7-8 layers, and the loofah sponge network structure layer is provided with 1-6 layers; the composite material film layer and the loofah sponge network structure layer are arranged in a layered and spaced mode.
As one of the preferable modes of the invention, the PA 6-citric acid blend is prepared by mixing PA6 and citric acid according to the mass ratio of 1: 0.2.
In a preferred embodiment of the present invention, the dispersant is a mixture of stearic acid, calcium stearate, and a zirconate coupling agent in a mass ratio of 1:1: 0.5.
As one of the preferable modes of the invention, the adhesive is formed by mixing carboxymethylcellulose and a rare earth nucleating agent WBG-II according to the mass ratio of 3: 1.
In a preferred embodiment of the present invention, the coupling agent is a silane coupling agent KH 560-ethanol solution, and KH 560: the ratio of the absolute ethyl alcohol is 1: 10.
A preparation method of the reinforced fiber polymer composite wallboard with the natural network framework comprises the following steps:
(1) pretreatment of pine cone fibers:
firstly, crushing pine cones of agricultural and forestry wastes, then soaking the crushed pine cones in tap water, and repeatedly washing the pine cones with running water; naturally airing, and drying the rice hulls to enable the water content of the rice hulls to be lower than 3%; finally, crushing pine nuts to obtain pine nut powder;
secondly, putting the pine cone powder into a coupling agent for soaking treatment, and then stirring for 25-35 min at the temperature of 45-55 ℃;
(2) pretreating natural loofah sponge network fibers:
firstly, cutting natural loofah into blocky loofah sponge, and then selecting a single-layer network-shaped structure with fibers arranged in a unidirectional mode on the innermost layer as a subsequent processing object;
secondly, adding the adhesion agent into an acetone solution, magnetically stirring for 2.5-3.5 hours under the condition of water bath at the temperature of 45-55 ℃, and then carrying out ultrasonic treatment for 25-35 min to form a treatment solution;
immersing the reticular structure of the loofah sponge obtained in the step one into the treatment solution obtained in the step two, and stirring; after stirring, taking out the loofah net structure and drying;
(3) preparation of composite materials
Weighing a PA 6-citric acid mixture, placing the mixture in an internal mixer for shearing and mixing, wherein the internal mixing temperature is 220-240 ℃, the time is 5-15 min, and the rotating speed is 20-60 rpm;
secondly, mixing the pine nut powder obtained in the step (1) with a dispersing agent, adding the mixture into the internal mixer, and continuously carrying out internal mixing for 10-20 min under the same conditions; after banburying is finished, crushing the banburied composite material to obtain composite material particles;
(4) wallboard preparation
Putting the composite material particles obtained in the step (3) into a mold, preheating at 220-240 ℃ for 5-15 min, and hot-pressing under the pressure of 8-12 MPa for 8-12 min to respectively prepare each composite material film layer; meanwhile, placing the loofah sponge net obtained in the step (2) on a hot press for shaping and thickness-fixing treatment, wherein the hot pressing condition is 125-135 ℃ and the time is 3-7 min, so as to prepare each loofah sponge net structure layer;
secondly, laminating the prepared loofah sponge network structure layer and the composite material thin film layer in sequence according to a target sequence by using a laminating mode, placing the loofah sponge network structure layer and the composite material thin film layer in a mold, preheating for 5-15 min at the temperature of 220-240 ℃, and hot-pressing for 8-12 min under the pressure of 8-12 MPa; wherein, the composite material film layer and the loofah sponge network structure layer are paved at intervals;
taking out the material, and curing at room temperature;
and fourthly, plating a waterproof film on the maintained material, and then carrying out veneering treatment to obtain the composite wallboard required by the target.
In a preferred embodiment of the present invention, in the step (1), the rice hulls are dried by an air-blowing drying oven; crushing pine nuts by using a universal crusher, and screening by using a 100-mesh screen to obtain pine nut powder; in the step (2), drying the taken loofah mesh structure by using a vacuum drying oven; in the step (3), after banburying is finished, crushing the banburied composite material by using a crusher to obtain composite material particles with the particle size of less than or equal to 100 meshes.
In a preferred embodiment of the present invention, in the step (2), the acetone solution has a water content of 60; in the step (3), 60% of PA 6-citric acid mixture is weighed and banburied.
In a preferred embodiment of the present invention, in the first step of the step (4), the mold has a thickness of 1mm and a size of 10X 10 cm; in the second step of the step (4), the thickness of the die is 3mm, and the size of the die is 10 multiplied by 10 cm.
Compared with the prior art, the invention has the advantages that:
(1) according to the invention, the natural fiber network structure with certain strength is embedded in the traditional natural fiber polymer composite material, so that the mechanical property and the dimensional stability of the traditional fiber polymer composite material are improved, the processing and development method of the composite material is simple, and the cost of the material is reduced;
(2) according to the invention, firstly, a silane coupling agent ethanol solution is used for carrying out graft modification treatment on the fibers, and then a composite dispersing agent stearic acid-calcium stearate-zirconate coupling agent is added, so that the interface compatibility between the fibers and a matrix and the dispersibility of the filler are improved, and the improvement of various performances of a single-layer structure in a layered mechanism is facilitated, thereby integrally improving the mechanical strength and the dimensional stability of the composite material; meanwhile, by utilizing carboxymethyl cellulose and a rare earth nucleating agent, on one hand, the interface combination between layers is improved when a laminating technology is utilized; on the other hand, a large number of hydroxyl groups shown by the natural fibers and amide groups in the PA6 matrix are promoted to form a large number of network structures connected by hydrogen bonds, so that the aging resistance, the impact resistance and the mechanical strength of the composite material are greatly improved;
(3) according to the invention, citric acid and PA6 are used for modification treatment, so that the toughness and ductility of the PA6 matrix are improved;
(4) the invention takes natural loofah sponge network fiber and waste pine nut powder as raw materials, and has the advantages of wide raw material source, low cost and environmental protection;
(5) the natural loofah sponge network fiber is combined with the porosity of the natural loofah sponge network fiber, a multi-layer structure design method is adopted, the natural loofah sponge network fiber is used for preparing the home decoration material wallboard, the sound absorption characteristic of the composite material can be improved to a certain extent, and the indoor living environment is optimized.
Drawings
Fig. 1 is a structural, layer-by-layer display view of a reinforced fiber polymer composite wallboard with a natural network backbone of example 1;
fig. 2 is a structural layer display view of a reinforced fiber polymer composite wallboard with a natural network backbone of example 2;
fig. 3 is a structural layer display view of the reinforced fiber polymer composite wallboard with natural network backbone of example 3;
fig. 4 is a structural layered display of the reinforced fiber polymer composite wallboard with natural network backbone of example 4.
Detailed Description
The following examples are given for the detailed implementation and specific operation of the present invention, but the scope of the present invention is not limited to the following examples.
Example 1
As shown in fig. 1, the reinforced fiber polymer composite wallboard with a natural network skeleton of the present embodiment includes a composite material film layer and a loofah sponge network structure layer. The composite material film layer is provided with eight layers, and each layer comprises the following raw materials in parts by weight: 50 parts of PA 6-citric acid blend, 40 parts of pine nut powder, 2 parts of a dispersing agent and 1 part of a coupling agent. The loofah sponge network structure layer is provided with a layer, is specifically embedded in the middle of the eight composite material thin film layers, and comprises the following raw materials in parts by weight: 4 parts of loofah sponge network fiber and 1 part of adhesive.
Further, in this embodiment, the PA 6-citric acid blend is formed by mixing PA6 and citric acid according to a mass ratio of 1: 0.2.
Further, in the embodiment, the dispersant is formed by mixing stearic acid, calcium stearate and a zirconate coupling agent according to a mass ratio of 1:1: 0.5.
Further, in the embodiment, the adhesive is formed by mixing carboxymethyl cellulose and a rare earth nucleating agent WBG-II according to a mass ratio of 3: 1.
Further, in this example, the coupling agent was a silane coupling agent KH 560-ethanol solution, and KH 560: the ratio of the absolute ethyl alcohol is 1: 10.
The preparation method of the composite wallboard comprises the following steps:
(1) pretreatment of pine cone fibers:
firstly, preliminarily crushing pine cones which are agricultural and forestry wastes, soaking the preliminarily crushed pine cones in tap water for 24 hours in order to reduce dirt and impurities in the pine cones, and repeatedly washing the pine cones with running water for 2 times; naturally drying the rice hulls by using an air-blast drying oven at 105 ℃ for 24 hours after the rice hulls are naturally dried, so that the water content of the rice hulls is lower than 3%; finally, crushing pine nuts by using a universal crusher, and screening by using a 100-mesh screen to obtain pine nut powder;
secondly, putting 100-mesh pine cone powder into a silane coupling agent KH 560-ethanol solution for soaking treatment according to the mass ratio of 1:2, and then stirring for 25min at the temperature of 45 ℃;
(2) pretreating natural loofah sponge network fibers:
cutting pre-washed and vacuum-dried natural loofah into blocky loofah with proper size, removing a compact layer on the surface and a secondary outer layer in the middle, and only keeping a single-layer network structure with fibers arranged in a unidirectional mode on the innermost layer;
secondly, adding carboxymethyl cellulose and a rare earth nucleating agent WBG-II into an acetone solution (with the water content of 60) according to a mass ratio, magnetically stirring for 2.5 hours under the condition of water bath at the temperature of 45 ℃, and then carrying out ultrasonic treatment for 25 minutes to form a uniform and stable treatment solution;
immersing the loofah sponge net structure obtained in the step (i) into the treatment solution obtained in the step (ii), and then stirring for 3 hours at the rotating speed of 300rpm by using a planetary stirrer; after stirring, taking out the loofah sponge net structure, putting the loofah sponge net structure into a vacuum drying oven, and drying for 24 hours at the temperature of 80 ℃;
(3) preparation of composite materials
Weighing 60% of PA 6-citric acid mixture, placing the mixture in an internal mixer for shearing and mixing, wherein the internal mixing temperature is 220 ℃, the time is 5min, and the rotating speed is 20 rpm;
secondly, mixing the pine nut powder obtained in the step (1) with a dispersing agent, adding the mixture into the internal mixer, and continuously carrying out internal mixing for 10min under the same conditions; after banburying is finished, crushing the banburied composite material to obtain composite material particles with smaller particle size (less than or equal to 100 meshes);
(4) wallboard preparation
Putting the composite material particles obtained in the step (3) into a die with the thickness of 1mm and the size of 10 multiplied by 10cm, preheating for 5min at the temperature of 220 ℃, hot-pressing for 8min under the pressure of 8MPa, and respectively preparing each composite material film layer with the thickness of 1 mm; meanwhile, placing the loofah sponge net obtained in the step (2) on a hot press for shaping and thickness-fixing treatment, wherein the hot pressing condition is 125 ℃ and 3min, so as to prepare each loofah sponge net structure layer;
secondly, laminating the prepared loofah sponge network structure layer and the composite material thin film layer in sequence according to a target sequence by using a laminating mode, placing the loofah sponge network structure layer and the composite material thin film layer in a mold with the thickness of 3mm and the size of 10 multiplied by 10cm, preheating for 5min at the temperature of 220 ℃, and hot-pressing for 8min under the pressure of 8 MPa; wherein, the composite material film layer and the loofah sponge network structure layer are paved at intervals;
taking out the material, and curing at room temperature for 72 h;
and fourthly, plating a waterproof film on the maintained material, and then carrying out veneering treatment to obtain the composite wallboard required by the target.
Example 2
As shown in fig. 2, the reinforced fiber polymer composite wallboard with a natural network skeleton of the present embodiment includes a composite material film layer and a loofah sponge network structure layer stacked and spaced with the loofah sponge network structure layer. The composite material film layer is provided with seven layers, and each layer comprises the following raw materials in parts by weight: 55 parts of PA 6-citric acid blend, 45 parts of pine cone powder, 2.5 parts of a dispersing agent and 2 parts of a coupling agent. The loofah sponge network structure layer is provided with two layers, and is respectively embedded between a third layer and a fourth layer of composite material thin film layers and between a fourth layer and a fifth layer of composite material thin film layers (named as a first layer and a second layer according to the sequence from top to bottom), and each layer respectively comprises the following raw materials in parts by weight: 5 parts of loofah sponge network fiber and 3 parts of adhesive.
Further, in this embodiment, the PA 6-citric acid blend is formed by mixing PA6 and citric acid according to a mass ratio of 1: 0.2.
Further, in the embodiment, the dispersant is formed by mixing stearic acid, calcium stearate and a zirconate coupling agent according to a mass ratio of 1:1: 0.5.
Further, in the embodiment, the adhesive is formed by mixing carboxymethyl cellulose and a rare earth nucleating agent WBG-II according to a mass ratio of 3: 1.
Further, in this example, the coupling agent was a silane coupling agent KH 560-ethanol solution, and KH 560: the ratio of the absolute ethyl alcohol is 1: 10.
The preparation method of the composite wallboard comprises the following steps:
(1) pretreatment of pine cone fibers:
firstly, preliminarily crushing pine cones which are agricultural and forestry wastes, soaking the preliminarily crushed pine cones in tap water for 24 hours in order to reduce dirt and impurities in the pine cones, and repeatedly washing the pine cones for 3 times by using running water; naturally drying the rice hulls by using an air-blast drying oven at 105 ℃ for 24 hours after the rice hulls are naturally dried, so that the water content of the rice hulls is lower than 3%; finally, crushing pine nuts by using a universal crusher, and screening by using a 100-mesh screen to obtain pine nut powder;
secondly, putting 100-mesh pine cone powder into a silane coupling agent KH 560-ethanol solution for soaking treatment according to the mass ratio of 1:2, and then stirring for 30min at the temperature of 50 ℃;
(2) pretreating natural loofah sponge network fibers:
cutting pre-washed and vacuum-dried natural loofah into blocky loofah with proper size, removing a compact layer on the surface and a secondary outer layer in the middle, and only keeping a single-layer network structure with fibers arranged in a unidirectional mode on the innermost layer;
secondly, adding carboxymethyl cellulose and a rare earth nucleating agent WBG-II into an acetone solution (with the water content of 60) according to a mass ratio, magnetically stirring for 23 hours under the condition of a water bath at the temperature of 50 ℃, and then performing ultrasonic treatment for 30 minutes to form a uniform and stable treatment solution;
immersing the loofah sponge net structure obtained in the step (i) into the treatment solution obtained in the step (ii), and then stirring for 3 hours at the rotating speed of 300rpm by using a planetary stirrer; after stirring, taking out the loofah sponge net structure, putting the loofah sponge net structure into a vacuum drying oven, and drying for 24 hours at the temperature of 80 ℃;
(3) preparation of composite materials
Weighing 60% of PA 6-citric acid mixture, placing the mixture in an internal mixer for shearing and mixing, wherein the internal mixing temperature is 230 ℃, the time is 10min, and the rotating speed is 40 rpm;
secondly, mixing the pine nut powder obtained in the step (1) with a dispersing agent, adding the mixture into the internal mixer, and continuously carrying out internal mixing for 15min under the same conditions; after banburying is finished, crushing the banburied composite material to obtain composite material particles with smaller particle size (less than or equal to 100 meshes);
(4) wallboard preparation
Putting the composite material particles obtained in the step (3) into a die with the thickness of 1mm and the size of 10 multiplied by 10cm, preheating for 10min at the temperature of 230 ℃, and hot-pressing for 10min under the pressure of 10MPa to respectively prepare each composite material film layer with the thickness of 1 mm; meanwhile, placing the loofah sponge net obtained in the step (2) on a hot press for shaping and thickness-fixing treatment, wherein the hot pressing condition is 130 ℃ and 5min, so as to prepare each loofah sponge net structure layer;
secondly, laminating the prepared loofah sponge network structure layer and the composite material thin film layer in sequence according to a target sequence by utilizing a laminating mode, placing the loofah sponge network structure layer and the composite material thin film layer in a mold with the thickness of 3mm and the size of 10 multiplied by 10cm, preheating for 10min at the temperature of 230 ℃, and hot-pressing for 10min under the pressure of 10 MPa; wherein, the composite material film layer and the loofah sponge network structure layer are paved at intervals;
taking out the material, and curing at room temperature for 72 h;
and fourthly, plating a waterproof film on the maintained material, and then carrying out veneering treatment to obtain the composite wallboard required by the target.
Example 3
As shown in fig. 3, the reinforced fiber polymer composite wallboard with a natural network skeleton of the present embodiment includes a composite material film layer and a loofah sponge network structure layer stacked and spaced with the loofah sponge network structure layer. The composite material film layer is provided with seven layers, and each layer comprises the following raw materials in parts by weight: 58 parts of PA 6-citric acid blend, 48 parts of pine cone powder, 2.8 parts of dispersing agent and 2.5 parts of coupling agent. The loofah sponge network structure layer is provided with four layers which are respectively embedded between a second layer and a third layer composite material thin layer, between a third layer and a fourth layer composite material thin layer, between a fourth layer and a fifth layer composite material thin layer and between a fifth layer and a sixth layer composite material thin layer (named as a first layer and a second layer), and each layer comprises the following raw materials in parts by weight: 7 parts of loofah sponge network fiber and 5 parts of adhesive.
Further, in this embodiment, the PA 6-citric acid blend is formed by mixing PA6 and citric acid according to a mass ratio of 1: 0.2.
Further, in the embodiment, the dispersant is formed by mixing stearic acid, calcium stearate and a zirconate coupling agent according to a mass ratio of 1:1: 0.5.
Further, in the embodiment, the adhesive is formed by mixing carboxymethyl cellulose and a rare earth nucleating agent WBG-II according to a mass ratio of 3: 1.
Further, in this example, the coupling agent was a silane coupling agent KH 560-ethanol solution, and KH 560: the ratio of the absolute ethyl alcohol is 1: 10.
The preparation method of the composite wallboard comprises the following steps:
(1) pretreatment of pine cone fibers:
firstly, preliminarily crushing pine cones which are agricultural and forestry wastes, soaking the preliminarily crushed pine cones in tap water for 24 hours in order to reduce dirt and impurities in the pine cones, and repeatedly washing the pine cones for 3 times by using running water; naturally drying the rice hulls by using an air-blast drying oven at 105 ℃ for 24 hours after the rice hulls are naturally dried, so that the water content of the rice hulls is lower than 3%; finally, crushing pine nuts by using a universal crusher, and screening by using a 100-mesh screen to obtain pine nut powder;
secondly, putting 100-mesh pine cone powder into a silane coupling agent KH 560-ethanol solution for soaking treatment according to the mass ratio of 1:2, and then stirring for 30min at the temperature of 50 ℃;
(2) pretreating natural loofah sponge network fibers:
cutting pre-washed and vacuum-dried natural loofah into blocky loofah with proper size, removing a compact layer on the surface and a secondary outer layer in the middle, and only keeping a single-layer network structure with fibers arranged in a unidirectional mode on the innermost layer;
secondly, adding carboxymethyl cellulose and a rare earth nucleating agent WBG-II into an acetone solution (with the water content of 60) according to a mass ratio, magnetically stirring for 3 hours under the condition of a water bath at the temperature of 50 ℃, and then performing ultrasonic treatment for 30 minutes to form a uniform and stable treatment solution;
immersing the loofah sponge net structure obtained in the step (i) into the treatment solution obtained in the step (ii), and then stirring for 3 hours at the rotating speed of 300rpm by using a planetary stirrer; after stirring, taking out the loofah sponge net structure, putting the loofah sponge net structure into a vacuum drying oven, and drying for 24 hours at the temperature of 80 ℃;
(3) preparation of composite materials
Weighing 60% of PA 6-citric acid mixture, placing the mixture in an internal mixer for shearing and mixing, wherein the internal mixing temperature is 230 ℃, the time is 10min, and the rotating speed is 40 rpm;
secondly, mixing the pine nut powder obtained in the step (1) with a dispersing agent, adding the mixture into the internal mixer, and continuously carrying out internal mixing for 15min under the same conditions; after banburying is finished, crushing the banburied composite material to obtain composite material particles with smaller particle size (less than or equal to 100 meshes);
(4) wallboard preparation
Putting the composite material particles obtained in the step (3) into a die with the thickness of 1mm and the size of 10 multiplied by 10cm, preheating for 10min at the temperature of 230 ℃, and hot-pressing for 10min under the pressure of 10MPa to respectively prepare each composite material film layer with the thickness of 1 mm; meanwhile, placing the loofah sponge net obtained in the step (2) on a hot press for shaping and thickness-fixing treatment, wherein the hot pressing condition is 130 ℃ and 5min, so as to prepare each loofah sponge net structure layer;
secondly, laminating the prepared loofah sponge network structure layer and the composite material thin film layer in sequence according to a target sequence by using a laminating mode, placing the loofah sponge network structure layer and the composite material thin film layer in a mold with the thickness of 3mm and the size of 10 multiplied by 10cm, preheating for 10min at the temperature of 220-240 ℃, and hot-pressing for 10min under the pressure of 10 MPa; wherein, the composite material film layer and the loofah sponge network structure layer are paved at intervals;
taking out the material, and curing at room temperature for 72 h;
and fourthly, plating a waterproof film on the maintained material, and then carrying out veneering treatment to obtain the composite wallboard required by the target.
Example 4
As shown in fig. 4, the reinforced fiber polymer composite wallboard with a natural network skeleton of the present embodiment includes a composite material film layer and a loofah sponge network structure layer stacked and spaced with the loofah sponge network structure layer. The composite material film layer is provided with seven layers, and each layer comprises the following raw materials in parts by weight: 60 parts of PA 6-citric acid blend, 50 parts of pine nut powder, 3 parts of a dispersing agent and 3 parts of a coupling agent. The loofah sponge network structure layer is provided with six layers which are respectively embedded between every two composite material thin layers, and each layer comprises the following raw materials in parts by weight: 8 parts of loofah sponge network fiber and 6 parts of adhesive.
Further, in this embodiment, the PA 6-citric acid blend is formed by mixing PA6 and citric acid according to a mass ratio of 1: 0.2.
Further, in the embodiment, the dispersant is formed by mixing stearic acid, calcium stearate and a zirconate coupling agent according to a mass ratio of 1:1: 0.5.
Further, in the embodiment, the adhesive is formed by mixing carboxymethyl cellulose and a rare earth nucleating agent WBG-II according to a mass ratio of 3: 1.
Further, in this example, the coupling agent was a silane coupling agent KH 560-ethanol solution, and KH 560: the ratio of the absolute ethyl alcohol is 1: 10.
The preparation method of the composite wallboard comprises the following steps:
(1) pretreatment of pine cone fibers:
firstly, preliminarily crushing pine cones which are agricultural and forestry wastes, soaking the preliminarily crushed pine cones in tap water for 24 hours in order to reduce dirt and impurities in the pine cones, and repeatedly washing the pine cones with running water for 2-4 times; naturally drying the rice hulls by using an air-blast drying oven at 105 ℃ for 24 hours after the rice hulls are naturally dried, so that the water content of the rice hulls is lower than 3%; finally, crushing pine nuts by using a universal crusher, and screening by using a 100-mesh screen to obtain pine nut powder;
secondly, putting 100-mesh pine cone powder into a silane coupling agent KH 560-ethanol solution for soaking treatment according to the mass ratio of 1:2, and then stirring for 35min at the temperature of 55 ℃;
(2) pretreating natural loofah sponge network fibers:
cutting pre-washed and vacuum-dried natural loofah into blocky loofah with proper size, removing a compact layer on the surface and a secondary outer layer in the middle, and only keeping a single-layer network structure with fibers arranged in a unidirectional mode on the innermost layer;
secondly, adding carboxymethyl cellulose and a rare earth nucleating agent WBG-II into an acetone solution (with the water content of 60) according to a mass ratio, magnetically stirring for 3.5 hours under the condition of a water bath at the temperature of 55 ℃, and then carrying out ultrasonic treatment for 35min to form a uniform and stable treatment solution;
immersing the loofah sponge net structure obtained in the step (i) into the treatment solution obtained in the step (ii), and then stirring for 3 hours at the rotating speed of 300rpm by using a planetary stirrer; after stirring, taking out the loofah sponge net structure, putting the loofah sponge net structure into a vacuum drying oven, and drying for 24 hours at the temperature of 80 ℃;
(3) preparation of composite materials
Weighing 60% of PA 6-citric acid mixture, placing the mixture in an internal mixer for shearing and mixing, wherein the internal mixing temperature is 240 ℃, the time is 15min, and the rotating speed is 60 rpm;
secondly, mixing the pine nut powder obtained in the step (1) with a dispersing agent, adding the mixture into the internal mixer, and continuously carrying out internal mixing for 20min under the same conditions; after banburying is finished, crushing the banburied composite material to obtain composite material particles with smaller particle size (less than or equal to 100 meshes);
(4) wallboard preparation
Putting the composite material particles obtained in the step (3) into a die with the thickness of 1mm and the size of 10 multiplied by 10cm, preheating for 15min at the temperature of 240 ℃, hot-pressing for 12min under the pressure of 12MPa, and respectively preparing each composite material film layer with the thickness of 1 mm; meanwhile, placing the loofah sponge net obtained in the step (2) on a hot press for shaping and thickness-fixing treatment, wherein the hot pressing condition is 135 ℃ and 7min, so as to prepare each loofah sponge net structure layer;
secondly, laminating the prepared loofah sponge network structure layer and the composite material thin film layer in sequence according to a target sequence by using a laminating mode, placing the loofah sponge network structure layer and the composite material thin film layer in a mold with the thickness of 3mm and the size of 10 multiplied by 10cm, preheating for 15min at the temperature of 240 ℃, and hot-pressing for 12min under the pressure of 12 MPa; wherein, the composite material film layer and the loofah sponge network structure layer are paved at intervals;
taking out the material, and curing at room temperature for 72 h;
and fourthly, plating a waterproof film on the maintained material, and then carrying out veneering treatment to obtain the composite wallboard required by the target.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Example 5
The performance test results of the reinforced fiber polymer composite wallboard with the natural network framework in the above examples 1 to 4 of this embodiment.
The reinforced fiber polymer composite wallboard with the corresponding natural network framework is prepared according to the raw material formula and the preparation method of each embodiment, and the samples are prepared and tested respectively.
The results of the various performance tests are shown in table 1. Table 1 shows that the dimensional stability, the surface property, the water absorption, the mechanical property, the formaldehyde emission and the like of the reinforced fiber polymer composite wallboard of the natural network framework are respectively measured according to LY/T1700-2007, GB/T24137-2009, GB/T9341-2008 and ASTM D570-2005, the test results meet the requirements of various standards on the performance of the wallboard, and the specific results are as follows.
Table 1 performance test results of reinforced fiber polymer composite wallboard with natural network backbone of each example
Figure BDA0003270024530000161

Claims (10)

1. A reinforced fiber polymer composite wallboard with a natural network framework is characterized by comprising a composite material film layer and a loofah sponge network structure layer; the composite material film layer is provided with a plurality of layers, and each layer comprises the following raw materials in parts by weight: 50-60 parts of PA 6-citric acid blend, 40-50 parts of pine nut powder, 2-3 parts of a dispersing agent and 1-3 parts of a coupling agent; the loofah sponge network structure layer is embedded between the composite material thin layers, and each layer comprises the following raw materials in parts by weight: 4-8 parts of loofah sponge network fiber and 1-6 parts of an adhesive.
2. The reinforced fiber polymer composite wallboard with the natural network framework as claimed in claim 1, wherein the composite material film layer is provided with 7-8 layers, and the loofah sponge network structure layer is provided with 1-6 layers; the composite material film layer and the loofah sponge network structure layer are arranged in a layered and spaced mode.
3. The reinforced fiber polymer composite wallboard with natural network framework of claim 1, wherein the PA 6-citric acid blend is formed by mixing PA6 and citric acid according to the mass ratio of 1: 0.2.
4. The reinforced fiber polymer composite wallboard with natural network framework of claim 1, wherein the dispersant is formed by mixing stearic acid, calcium stearate and zirconate coupling agent according to the mass ratio of 1:1: 0.5.
5. The reinforced fiber polymer composite wallboard with natural network framework and the preparation method of the reinforced fiber polymer composite wallboard with natural network framework as claimed in claim 1, wherein the adhesive is formed by mixing carboxymethylcellulose and rare earth nucleating agent WBG-II according to a mass ratio of 3: 1.
6. The reinforced fiber polymer composite wallboard with natural network framework as claimed in claim 1, wherein the coupling agent is silane coupling agent KH 560-ethanol solution, and KH 560: the ratio of the absolute ethyl alcohol is 1: 10.
7. A method for preparing the reinforced fiber polymer composite wallboard with the natural network framework as claimed in any one of claims 1 to 6, wherein the method comprises the following steps:
(1) pretreatment of pine cone fibers:
firstly, crushing pine cones of agricultural and forestry wastes, then soaking the crushed pine cones in tap water, and repeatedly washing the pine cones with running water; naturally airing, and drying the rice hulls to enable the water content of the rice hulls to be lower than 3%; finally, crushing pine nuts to obtain pine nut powder;
secondly, putting the pine cone powder into a coupling agent for soaking treatment, and then stirring for 25-35 min at the temperature of 45-55 ℃;
(2) pretreating natural loofah sponge network fibers:
firstly, cutting natural loofah into blocky loofah sponge, and then selecting a single-layer network-shaped structure with fibers arranged in a unidirectional mode on the innermost layer as a subsequent processing object;
secondly, adding the adhesion agent into an acetone solution, magnetically stirring for 2.5-3.5 hours under the condition of water bath at the temperature of 45-55 ℃, and then carrying out ultrasonic treatment for 25-35 min to form a treatment solution;
immersing the reticular structure of the loofah sponge obtained in the step one into the treatment solution obtained in the step two, and stirring; after stirring, taking out the loofah net structure and drying;
(3) preparation of composite materials
Weighing a PA 6-citric acid mixture, placing the mixture in an internal mixer for shearing and mixing, wherein the internal mixing temperature is 220-240 ℃, the time is 5-15 min, and the rotating speed is 20-60 rpm;
secondly, mixing the pine nut powder obtained in the step (1) with a dispersing agent, adding the mixture into the internal mixer, and continuously carrying out internal mixing for 10-20 min under the same conditions; after banburying is finished, crushing the banburied composite material to obtain composite material particles;
(4) wallboard preparation
Putting the composite material particles obtained in the step (3) into a mold, preheating at 220-240 ℃ for 5-15 min, and hot-pressing under the pressure of 8-12 MPa for 8-12 min to respectively prepare each composite material film layer; meanwhile, placing the loofah sponge net obtained in the step (2) on a hot press for shaping and thickness-fixing treatment, wherein the hot pressing condition is 125-135 ℃ and the time is 3-7 min, so as to prepare each loofah sponge net structure layer;
secondly, laminating the prepared loofah sponge network structure layer and the composite material thin film layer in sequence according to a target sequence by using a laminating mode, placing the loofah sponge network structure layer and the composite material thin film layer in a mold, preheating for 5-15 min at the temperature of 220-240 ℃, and hot-pressing for 8-12 min under the pressure of 8-12 MPa; wherein, the composite material film layer and the loofah sponge network structure layer are paved at intervals;
taking out the material, and curing at room temperature;
and fourthly, plating a waterproof film on the maintained material, and then carrying out veneering treatment to obtain the composite wallboard required by the target.
8. The method for preparing the reinforced fiber polymer composite wallboard with the natural network framework as claimed in claim 7, wherein in the step (1), rice hulls are dried by using an air blowing drying oven; crushing pine nuts by using a universal crusher, and screening by using a 100-mesh screen to obtain pine nut powder; in the step (2), drying the taken loofah mesh structure by using a vacuum drying oven; in the step (3), after banburying is finished, crushing the banburied composite material by using a crusher to obtain composite material particles with the particle size of less than or equal to 100 meshes.
9. The method for preparing the reinforced fiber polymer composite wallboard with the natural network skeleton of claim 7, wherein in the step (2), the water content of the acetone solution is 60; in the step (3), 60% of PA 6-citric acid mixture is weighed and banburied.
10. The method for preparing a reinforced fiber polymer composite wallboard with a natural network skeleton as claimed in claim 7, wherein in the (4) step (1), the thickness of the mould is 1mm, and the size is 10 x 10 cm; in the second step of the step (4), the thickness of the die is 3mm, and the size of the die is 10 multiplied by 10 cm.
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