CN115260780A - Environment-friendly flame-retardant high-strength fiber composite board - Google Patents
Environment-friendly flame-retardant high-strength fiber composite board Download PDFInfo
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Abstract
The invention discloses an environment-friendly flame-retardant high-strength fiber composite board, and relates to the technical field of new materials. The invention firstly sprays the fold layer dispersion liquid on the surface of the polyurethane film, and dries and carbonizes the sprayed polyurethane film to prepare the modified polyurethane film, then the aminated carboxymethyl chitosan reacts with the silicon dioxide to prepare the modified silicon dioxide, the modified silicon dioxide is mixed with the epoxy resin and the phthalic anhydride, the mixture is vacuumized and injected into the modified polyurethane film, the modified epoxy resin is prepared after solidification, the modified epoxy resin is mixed with the pretreated wood fiber, and the calcium oxide, the ammonium acetate, the aminated carboxymethyl chitosan and the oxidized dextran are added, the mixture is obtained after stirring and mixing, and the environment-friendly flame-retardant high-strength fiber composite board is prepared after hot pressing the mixture for many times. The environment-friendly flame-retardant high-strength fiber composite board prepared by the invention has excellent mechanical property and flame retardance.
Description
Technical Field
The invention relates to the technical field of new materials, in particular to an environment-friendly flame-retardant high-strength fiber composite board.
Background
The natural fiber has small fiber density and high specific strength, and is developed as a reinforcing material, and a great deal of research and invention is already carried out. The natural fiber is a recyclable material, the growth cycle of the natural fiber is mostly 1-2 years, the material can be naturally degraded after being discarded after a period of time, and the natural fiber is used as a green environment-friendly material, and the development of the application capability of the material is continuously expanded. Many scientific achievements in Europe and America, japan and China also enter the practical popularization stage, and show good application prospects. At present, parts such as an instrument panel, a door inner panel, a ceiling, a trunk lining and the like of automotive interior parts and natural fiber composite materials are involved.
Patent 200810005276.3 adopts: wood chipping, fiber grinding, fiber sizing, fiber paving, prepressing, hot pressing, trimming, sanding and the like to obtain the wood fiber with the density of 0.25-0.45g/cm3The flame-retardant sheet material. The low-density fiber processed and formed by the patent has good performances of sound absorption, sound insulation and the like, and can be widely used as a door core of a wooden door, a core material of a partition wall and the like.
Chinese patent 200610039121.2 will make the required fibre of veneer layer, middle basic unit and precoat, according to veneer layer, the order of middle basic unit and precoat through lapping, the compound felt of acupuncture becomes, again through hot rolling shaping, the processing forms car ceiling panel, this fibrilia's use amount is great to can improve the quality of product through the hot-rolling pressing, but because the middle basic unit of material adds polyester fiber, the material does not bond completely, lead to the intensity of material lower, be unsuitable for the higher occasion of intensity.
The above patents all suffer from different problems, such as: the fiber board glued by the adhesive has high environmental pollution and is not suitable for being used in large quantities; the common fiber composite board has no flame retardant property; the traditional fiber composite board has low strength and cannot meet most use scenes, so that the use range of the fiber composite board is limited.
Disclosure of Invention
The invention aims to provide an environment-friendly flame-retardant high-strength fiber composite board and a preparation method thereof, and aims to solve the problems in the prior art.
The environment-friendly flame-retardant high-strength fiber composite board is characterized by mainly comprising the following raw material components in parts by weight: 60 to 80 parts of pretreated wood fiber, 3 to 8 parts of calcium oxide, 3 to 6 parts of ammonium acetate, 8 to 20 parts of modified epoxy resin, 5 to 12 parts of aminated carboxymethyl chitosan and 5 to 10 parts of oxidized dextran;
the modified epoxy resin is prepared by carbonizing a modified polyurethane film and coating a shape memory material on the surface of the carbonized modified polyurethane film.
As optimization, the modified polyurethane film is prepared by preparing a modified polyurethane film blank from the folded laminar object and the polyurethane film through a blowing expansion method, and carbonizing the modified polyurethane film blank in an inert gas atmosphere to prepare the modified polyurethane film; the folded laminar material is prepared by mixing and calcining titanium dihydride, aluminum powder and graphite powder, and then etching the mixture by hydrochloric acid and fluorine.
Preferably, the shape memory material is prepared by mixing epoxy resin E-51, phthalic anhydride and silicon dioxide loaded with aminated carboxymethyl chitosan, vacuumizing, injection molding and curing.
Preferably, the pretreated wood fiber is prepared by soaking the wood fiber in water, and then performing rubber grinding and sieving.
As optimization, the environment-friendly flame-retardant high-strength fiber composite board mainly comprises the following raw material components in parts by weight: 70 parts of pretreated wood fiber, 8 parts of calcium oxide, 5 parts of ammonium acetate, 12 parts of modified epoxy resin, 10 parts of aminated carboxymethyl chitosan and 10 parts of oxidized dextran.
As optimization, the preparation method of the environment-friendly flame-retardant high-strength fiber composite board mainly comprises the following preparation steps:
(1) Mixing the wrinkled laminar dispersion liquid with ethanol to obtain wrinkled laminar spraying liquid, fixing a polyurethane film on a funnel, sealing the outer side of the funnel, blowing air into the funnel at a constant speed, spraying the blown polyurethane film by using the wrinkled laminar spraying liquid when the polyurethane film is blown to a certain height, drying after spraying to obtain a modified polyurethane film blank, and carbonizing the modified polyurethane film blank in inert gas to obtain the modified polyurethane film;
(2) Mixing aminated carboxymethyl chitosan with water, adding silicon dioxide, stirring and mixing, adjusting the pH value to be alkaline, filtering, washing and drying to obtain modified silicon dioxide, mixing epoxy resin E-51 with phthalic anhydride, adding the modified silicon dioxide, heating, stirring and mixing to obtain epoxy resin E-51 mixture, vacuumizing the epoxy resin E-51 mixture, coating the mixture on the wrinkled surface of the modified polyurethane film obtained in the step (1), curing, crushing and sieving to obtain modified epoxy resin;
(3) Mixing and soaking wood fibers and water, filtering to obtain a pretreated wood fiber blank, carrying out colloid milling on the pretreated wood fiber blank, and sieving to obtain pretreated wood fibers;
(4) Mixing the pretreated wood fiber obtained in the step (3) with the modified epoxy resin obtained in the step (2), adding calcium oxide, ammonium acetate, aminated carboxymethyl chitosan and oxidized dextran, and stirring and mixing to obtain a mixture;
(5) And (4) hot-pressing the mixture obtained in the step (4) for multiple times to obtain the environment-friendly flame-retardant high-strength fiber composite board.
As optimization, the preparation method of the environment-friendly flame-retardant high-strength fiber composite board mainly comprises the following preparation steps:
(1) Mixing the wrinkled laminar dispersion liquid with absolute ethyl alcohol according to a volume ratio of 1 to 5 to obtain a wrinkled laminar spraying liquid, fixing a polyurethane film on a funnel with the diameter of 6-10cm, sealing the outer side of the polyurethane film, simultaneously blowing air into the funnel at a constant speed of 5-10mL/min, when the polyurethane film is blown to be 3-5cm, spraying the blown polyurethane film by using the wrinkled laminar spraying liquid with the mass of 8-15 times that of the polyurethane film, controlling the spraying speed to be 1-3mL/min, after the spraying is finished, obtaining a modified polyurethane film blank, drying the modified polyurethane film blank at the temperature of 60-80 ℃ for 20-40min, then placing the dried modified polyurethane film blank in a carbonization furnace, introducing nitrogen into the furnace at the speed of 30-80mL/min, discharging the dried modified polyurethane film blank at the temperature of 600-700 ℃ for 2h, and obtaining the modified polyurethane film blank;
(2) Mixing aminated carboxymethyl chitosan and water in a beaker according to the mass ratio of 1 to 10, adding silicon dioxide with the mass being 1 to 2 times that of the aminated carboxymethyl chitosan into the beaker, stirring and mixing for 2 hours, then adjusting the pH value of materials in the beaker to 13 by using a sodium hydroxide solution with the concentration being 1mol/L, filtering to obtain a modified silicon dioxide blank, washing the modified silicon dioxide blank with deionized water until the washing liquid is neutral, drying for 2 to 4 hours at the temperature of 80 ℃ to obtain modified silicon dioxide, mixing epoxy resin E-51 with phthalic anhydride according to the mass ratio of 5 to 2, adding modified silicon dioxide with the mass being 0.02 to 0.08 times that of epoxy resin E-51, stirring and mixing for 15 to 30min at the temperature of 60 to 70 ℃ to obtain an epoxy resin E-51 mixture, vacuumizing for 15min at the temperature of 80 ℃ to 15min, coating the epoxy resin E-51 mixture on the wrinkled surface of the modified polyurethane film obtained in the step (1), controlling the constant temperature of the epoxy resin E-51 mixture to be 3 min, heating for 2/5 hours, heating to 3 ℃ to 2 hours, heating to 3 ℃ and then heating to 100 ℃ to obtain the epoxy resin blank, and heating to 100 ℃ and heating to 2 hours, and then heating to obtain the epoxy resin blank, and heating to 100 ℃ after heating to 3 ℃ to 2 hours;
(3) Mixing and soaking wood fibers and water for 24 hours according to a mass ratio of 1 to 20 to 1, filtering to obtain a pretreated wood fiber blank, carrying out rubber grinding on the pretreated wood fiber blank for 3 hours, and sieving with a 100-mesh sieve to obtain pretreated wood fibers;
(4) Weighing the following components in percentage by mass: 70 parts of the pretreated wood fiber obtained in the step (3), 8 parts of calcium oxide, 5 parts of ammonium acetate, 12 parts of the modified epoxy resin obtained in the step (2), 10 parts of aminated carboxymethyl chitosan and 10 parts of oxidized dextran, mixing the pretreated wood fiber obtained in the step (3) and the modified epoxy resin obtained in the step (2) in a stirrer, adding the calcium oxide, the ammonium acetate, the aminated carboxymethyl chitosan and the oxidized dextran into the stirrer, and stirring and mixing to obtain a mixture;
(5) And (3) firstly pressing the mixture obtained in the step (4) for 5min under the conditions of the pressure of 1.5MPa and the temperature of 200 ℃, keeping the pressure, cooling to 80 ℃, pressing for 5min at constant temperature and constant pressure, then pressing for 5min at constant temperature and constant pressure under the conditions of the pressure of 3MPa and the temperature of 200 ℃, keeping the pressure, cooling to 80 ℃, continuing to press for 5min, finally pressing for 5min at constant temperature and constant pressure under the conditions of the pressure of 4.5MPa and the temperature of 200 ℃, cooling to room temperature, discharging, and thus obtaining the environment-friendly flame-retardant high-strength fiber composite board.
As an optimization, the preparation method of the wrinkled laminar dispersion in the step (1) comprises the steps of mixing titanium dihydride powder, aluminum powder and graphite powder in a molar ratio of 3; the thickness of the polyurethane film in the step (1) is 0.5 to 0.8mm.
Preferably, the preparation method of the aminated carboxymethyl chitosan in the steps (2) and (4) comprises the steps of mixing carboxymethyl chitosan with a phosphate buffer solution with the pH value of 5.0 according to the mass ratio of 1.
Preferably, the preparation method of the oxidized glucan in the step (4) comprises the following steps of mixing glucan and deionized water according to the mass ratio of 1:10, mixing, stirring and dissolving, adding a 100g/L potassium periodate solution with the mass of 2-5 times of that of the glucan, reacting for 5 hours at 25 ℃ in a dark condition, adding diethylene glycol with the mass of 0.1-0.2 time of that of the glucan to obtain an oxidized glucan mixture, dialyzing the oxidized glucan mixture in a dialysis bag with the molecular weight cutoff of 3500 for 72-96hours to obtain an oxidized glucan blank, and freeze-drying the oxidized glucan blank to obtain the oxidized glucan.
Compared with the prior art, the invention has the beneficial effects that:
the invention uses wood fiber as raw material when preparing environment-friendly flame-retardant high-strength fiber composite board, and adds calcium oxide, ammonium acetate, modified epoxy resin, aminated carboxymethyl chitosan and oxidized dextran into the product.
Firstly, wood fibers are used as raw materials to prepare the environment-friendly flame-retardant high-strength fiber composite board, the wood fibers can generate a large amount of furfural in the hot pressing process, and the furfural and hydrogen bonds among the wood fibers can jointly reinforce the wood fibers, so that the bonding force among the wood fibers is improved, and the strength of the product is further improved;
secondly, the aminated carboxymethyl chitosan, the oxidized glucan, the calcium oxide and the ammonium acetate are added into the product, and the ammonium acetate can be used as a catalyst for Schiff base reaction between the aminated carboxymethyl chitosan and the oxidized glucan, so that the Schiff base reaction between the aminated carboxymethyl chitosan and the oxidized glucan is promoted to form a viscous adhesive, and therefore the bonding force between fibers in the product is improved, and the strength of the product is improved; meanwhile, water is generated when the aminated carboxymethyl chitosan reacts with the oxidized glucan, calcium oxide can be changed into calcium hydroxide together with residual water in the wood fiber, a large amount of heat is released, ammonium acetate is quickly changed into acetic acid during hot pressing, the calcium acetate can further react with the calcium hydroxide to generate calcium acetate, the generated calcium acetate can be decomposed under the heat generated by the hot pressing and the reaction of the calcium oxide and the water, calcium carbonate filling is formed in the product, and the strength of the product is further improved;
furthermore, the modified epoxy resin added in the invention is a mixture of the shape memory material, the wrinkled laminar matter and the carbonaceous material, and a multi-time hot pressing method with different pressures is used during hot pressing, so that the shape memory material can be deformed for many times, and can be shrunk for many times after being cooled, and further the shape memory material, the wrinkled laminar matter and the carbonaceous material are dispersed in a product matrix, the strength and the flame retardant property of the product are improved, and the shape memory material can form a grinding effect on the aminated carboxymethyl chitosan and the oxidized dextran due to multi-time deformation and shrinkage, so that the reaction of the aminated carboxymethyl chitosan and the oxidized dextran is promoted; and because the initial shape of the shape memory material is corrugated, the shape memory material can be recovered to be corrugated at the last of the preparation of the product, the bonding force between wood fibers in the product is improved, and the strength is further improved.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, belong to the protection scope of the present invention.
In order to more clearly illustrate the method provided by the present invention, the following examples are used to describe in detail, and the test methods of the indexes of the environment-friendly flame-retardant high-strength fiber composite board manufactured in the following examples are as follows:
static bending strength: the static bending strength of the environment-friendly flame-retardant high-strength fiber composite board obtained in each example and the comparative product is measured according to GB/T11718.
Flame retardancy; and (4) measuring the limiting oxygen index of the environment-friendly flame-retardant high-strength fiber composite board obtained in each example and the comparative product.
Example 1
An environment-friendly flame-retardant high-strength fiber composite board mainly comprises the following components in parts by weight: 70 parts of pretreated wood fiber, 8 parts of calcium oxide, 5 parts of ammonium acetate, 12 parts of modified epoxy resin, 10 parts of aminated carboxymethyl chitosan and 10 parts of oxidized dextran.
The preparation method of the environment-friendly flame-retardant high-strength fiber composite board mainly comprises the following preparation steps:
(1) Mixing the folded laminar dispersion liquid with absolute ethyl alcohol according to a volume ratio of 1;
(2) Mixing aminated carboxymethyl chitosan and water in a mass ratio of 1: obtaining an epoxy resin E-51 mixture, vacuumizing the epoxy resin E-51 mixture for 15min at the temperature of 80 ℃, coating the epoxy resin E-51 mixture on the wrinkled surface of the modified polyurethane film obtained in the step (1), controlling the using amount of the epoxy resin E-51 mixture to be 4mL/g, heating the epoxy resin E-51 mixture for 1h at the temperature of 80 ℃, then heating the epoxy resin E-51 mixture to 100 ℃ at the heating rate of 2 ℃/min, heating the epoxy resin E-51 mixture for 3h at constant temperature, continuing heating the epoxy resin E-51 mixture to 150 ℃ at the heating rate of 2 ℃/min, keeping the temperature for 5h, finally heating the epoxy resin E-51 mixture to 180 ℃ at the heating rate of 2 ℃/min, keeping the temperature for 3h to obtain a modified epoxy resin blank, crushing the modified epoxy resin blank, and sieving the modified epoxy resin with a sieve of 5 meshes to obtain the modified epoxy resin;
(3) Mixing and soaking wood fibers and water for 24 hours according to a mass ratio of 1;
(4) Weighing the following components in sequence according to mass fraction: 70 parts of the pretreated wood fiber obtained in the step (3), 8 parts of calcium oxide, 5 parts of ammonium acetate, 12 parts of the modified epoxy resin obtained in the step (2), 10 parts of aminated carboxymethyl chitosan and 10 parts of oxidized dextran, mixing the pretreated wood fiber obtained in the step (3) and the modified epoxy resin obtained in the step (2) in a stirrer, adding the calcium oxide, the ammonium acetate, the aminated carboxymethyl chitosan and the oxidized dextran into the stirrer, and stirring and mixing to obtain a mixture;
(5) And (3) firstly pressing the mixture obtained in the step (4) for 5min under the conditions of the pressure of 1.5MPa and the temperature of 200 ℃, keeping the pressure, cooling to 80 ℃, pressing for 5min at constant temperature and constant pressure, then pressing for 5min at constant temperature and constant pressure under the conditions of the pressure of 3MPa and the temperature of 200 ℃, keeping the pressure, cooling to 80 ℃, continuing to press for 5min, finally pressing for 5min at constant temperature and constant pressure under the conditions of the pressure of 4.5MPa and the temperature of 200 ℃, cooling to room temperature, discharging, and thus obtaining the environment-friendly flame-retardant high-strength fiber composite board.
Optimally, the preparation method of the wrinkled laminar dispersion liquid in the step (1) comprises the steps of mixing titanium dihydride powder, aluminum powder and graphite powder according to a molar ratio of 3: 1.1; the thickness of the polyurethane film in the step (1) is 0.6mm.
Optimally, the preparation method of the aminated carboxymethyl chitosan in the step (2) and the step (4) comprises the steps of mixing carboxymethyl chitosan with phosphate buffer solution with the pH value of 5.0 according to the mass ratio of 1.
Preferably, the preparation method of the oxidized glucan in the step (4) comprises the following steps of mixing glucan and deionized water according to the mass ratio of 1:10, mixing, stirring for dissolving, adding 100g/L potassium periodate solution with the mass of 3 times of that of the glucan, reacting for 5 hours at 25 ℃ in a dark place, adding diethylene glycol with the mass of 0.1 time of that of the glucan to obtain an oxidized glucan mixture, dialyzing the oxidized glucan mixture in a dialysis bag with the molecular weight cutoff of 3500 for 72 hours to obtain an oxidized glucan blank, and freeze-drying the oxidized glucan blank to obtain the oxidized glucan.
Example 2
An environment-friendly flame-retardant high-strength fiber composite board mainly comprises the following components in parts by weight: 70 parts of pretreated wood fiber, 8 parts of calcium oxide, 5 parts of ammonium acetate, 12 parts of modified epoxy resin, 10 parts of aminated carboxymethyl chitosan and 10 parts of oxidized dextran.
The preparation method of the environment-friendly flame-retardant high-strength fiber composite board mainly comprises the following preparation steps:
(1) Mixing the folded laminar dispersion liquid with absolute ethyl alcohol according to a volume ratio of 1;
(2) Mixing epoxy resin E-51 with phthalic anhydride according to a mass ratio of 5 to 2, adding silicon dioxide which is 0.06 times of the mass of the epoxy resin E-51, stirring and mixing for 20min at a temperature of 65 ℃ to obtain an epoxy resin E-51 mixture, vacuumizing the epoxy resin E-51 mixture for 15min at a temperature of 80 ℃, coating the epoxy resin E-51 mixture on the wrinkled surface of the modified polyurethane film obtained in the step (1), controlling the using amount of the epoxy resin E-51 mixture to be 4mL/g, heating for 1h at a temperature of 80 ℃, then heating to 100 ℃ at a heating rate of 2 ℃/min, heating for 3h at a constant temperature, continuing heating to 150 ℃ at a heating rate of 2 ℃/min, keeping the temperature for 5h, finally heating to 180 ℃ at a heating rate of 2 ℃/min, carrying out heat preservation treatment for 3h to obtain a modified epoxy resin blank, crushing the modified epoxy resin blank, and sieving by a 5-mesh sieve to obtain modified epoxy resin;
(3) Mixing and soaking wood fibers and water for 24 hours according to a mass ratio of 1;
(4) Weighing the following components in percentage by mass: 70 parts of the pretreated wood fiber obtained in the step (3), 8 parts of calcium oxide, 5 parts of ammonium acetate, 12 parts of the modified epoxy resin obtained in the step (2), 10 parts of aminated carboxymethyl chitosan and 10 parts of oxidized dextran, mixing the pretreated wood fiber obtained in the step (3) and the modified epoxy resin obtained in the step (2) in a stirrer, adding the calcium oxide, the ammonium acetate, the aminated carboxymethyl chitosan and the oxidized dextran into the stirrer, and stirring and mixing to obtain a mixture;
(5) And (5) pressing the mixture obtained in the step (4) for 5min under the conditions of pressure of 1.5MPa and temperature of 200 ℃, maintaining the pressure, cooling to 80 ℃, pressing for 5min at constant temperature and constant pressure, then pressing for 5min at constant temperature and constant pressure under the conditions of pressure of 3MPa and temperature of 200 ℃, maintaining the pressure, cooling to 80 ℃, continuing to press for 5min, finally pressing for 5min at constant temperature and constant pressure under the conditions of pressure of 4.5MPa and temperature of 200 ℃, cooling to room temperature, and discharging to obtain the environment-friendly flame-retardant high-strength fiber composite board.
Optimally, the preparation method of the wrinkled laminar dispersion liquid in the step (1) comprises the steps of mixing titanium dihydride powder, aluminum powder and graphite powder according to a molar ratio of 3: 1.1; the thickness of the polyurethane film in the step (1) is 0.6mm.
Preferably, the preparation method of the aminated carboxymethyl chitosan in the steps (2) and (4) comprises the steps of mixing carboxymethyl chitosan with phosphate buffer solution with the pH value of 5.0 according to the mass ratio of 1 to 100, adding ethylenediamine with the mass of 2 times that of the carboxymethyl chitosan, adjusting the pH value to 5.5, adding 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride with the mass of 0.12 time that of the carboxymethyl chitosan, stirring for reaction to obtain an aminated carboxymethyl chitosan mixture, dialyzing the aminated carboxymethyl chitosan mixture in a dialysis bag with the molecular weight cutoff of 3400 for 20 hours to obtain an aminated carboxymethyl chitosan blank, and freeze-drying the aminated carboxymethyl chitosan blank to obtain the aminated carboxymethyl chitosan.
Preferably, the preparation method of the oxidized glucan in the step (4) comprises the following steps of mixing glucan and deionized water according to the mass ratio of 1:10, mixing, stirring for dissolving, adding a potassium periodate solution with the concentration of 100g/L and the mass of 3 times of that of the glucan, reacting for 5 hours at 25 ℃ in a dark condition, adding diethylene glycol with the mass of 0.1 time of that of the glucan to obtain an oxidized glucan mixture, dialyzing the oxidized glucan mixture in a dialysis bag with the molecular weight cutoff of 3500 for 72 hours to obtain an oxidized glucan blank, and freeze-drying the oxidized glucan blank to obtain the oxidized glucan.
Example 3
An environment-friendly flame-retardant high-strength fiber composite board mainly comprises the following components in parts by weight: 70 parts of pretreated wood fiber, 8 parts of calcium oxide, 5 parts of ammonium acetate, 12 parts of modified epoxy resin, 10 parts of aminated carboxymethyl chitosan and 10 parts of oxidized dextran.
The preparation method of the environment-friendly flame-retardant high-strength fiber composite board mainly comprises the following preparation steps:
(1) Mixing the silicon dioxide dispersion liquid with absolute ethyl alcohol according to a volume ratio of 1;
(2) Mixing aminated carboxymethyl chitosan and water in a beaker according to a mass ratio of 1:10, adding silicon dioxide which is 1.2 times of the mass of aminated carboxymethyl chitosan into the beaker, stirring and mixing for 2h, adjusting the pH value of materials in the beaker to 13 by using a sodium hydroxide solution with the concentration of 1mol/L, filtering to obtain a modified silicon dioxide blank, washing the modified silicon dioxide blank by using deionized water until the washing solution is neutral, drying for 3h at the temperature of 80 ℃ to obtain modified silicon dioxide, mixing epoxy resin E-51 with phthalic anhydride according to a mass ratio of 5:2, adding modified silicon dioxide which is 0.06 times of the mass of epoxy resin E-51, stirring and mixing for 20min at the temperature of 65 ℃ to obtain an epoxy resin E-51 mixture, vacuumizing the epoxy resin E-51 mixture for 15min at the temperature of 80 ℃, coating the epoxy resin E-51 mixture on the wrinkled surface of the modified film obtained in the step (1), controlling the use amount of the epoxy resin E-51 mixture to be 4mL/g, heating to the constant temperature of 80 ℃ for 15min, heating to 2 ℃/5 h, heating to obtain a modified epoxy resin wrinkled surface, heating to obtain a temperature-keeping blank, and heating to obtain a temperature-modified epoxy resin, and heating to 2 ℃/3 h, and heating to obtain a temperature-modified polyurethane wrinkled surface after heating to obtain a temperature-modified epoxy resin blank, wherein the epoxy resin blank, the epoxy resin is heated to obtain a temperature-modified polyurethane wrinkled rate of the epoxy resin, and the epoxy resin after heating rate of 2 ℃/3 h;
(3) Mixing and soaking wood fibers and water for 24 hours according to a mass ratio of 1;
(4) Weighing the following components in sequence according to mass fraction: 70 parts of the pretreated wood fiber obtained in the step (3), 8 parts of calcium oxide, 5 parts of ammonium acetate, 12 parts of the modified epoxy resin obtained in the step (2), 10 parts of aminated carboxymethyl chitosan and 10 parts of oxidized dextran, mixing the pretreated wood fiber obtained in the step (3) and the modified epoxy resin obtained in the step (2) in a stirrer, adding the calcium oxide, the ammonium acetate, the aminated carboxymethyl chitosan and the oxidized dextran into the stirrer, and stirring and mixing to obtain a mixture;
(5) And (3) firstly pressing the mixture obtained in the step (4) for 5min under the conditions of the pressure of 1.5MPa and the temperature of 200 ℃, keeping the pressure, cooling to 80 ℃, pressing for 5min at constant temperature and constant pressure, then pressing for 5min at constant temperature and constant pressure under the conditions of the pressure of 3MPa and the temperature of 200 ℃, keeping the pressure, cooling to 80 ℃, continuing to press for 5min, finally pressing for 5min at constant temperature and constant pressure under the conditions of the pressure of 4.5MPa and the temperature of 200 ℃, cooling to room temperature, discharging, and thus obtaining the environment-friendly flame-retardant high-strength fiber composite board.
As optimization, the preparation method of the silicon dioxide dispersion liquid in the step (1) comprises the steps of mixing nano silicon dioxide and water according to the mass ratio of 1; the thickness of the polyurethane film in the step (1) is 0.6mm.
Optimally, the preparation method of the aminated carboxymethyl chitosan in the step (2) and the step (4) comprises the steps of mixing carboxymethyl chitosan with phosphate buffer solution with the pH value of 5.0 according to the mass ratio of 1.
As an optimization, the preparation method of the oxidized dextran in the step (4) comprises the following steps of mixing dextran and deionized water according to a mass ratio of 1:10, mixing, stirring for dissolving, adding a potassium periodate solution with the concentration of 100g/L and the mass of 3 times of that of the glucan, reacting for 5 hours at 25 ℃ in a dark condition, adding diethylene glycol with the mass of 0.1 time of that of the glucan to obtain an oxidized glucan mixture, dialyzing the oxidized glucan mixture in a dialysis bag with the molecular weight cutoff of 3500 for 72 hours to obtain an oxidized glucan blank, and freeze-drying the oxidized glucan blank to obtain the oxidized glucan.
Example 4
An environment-friendly flame-retardant high-strength fiber composite board mainly comprises the following components in parts by weight: 70 parts of pretreated wood fiber, 8 parts of calcium oxide, 5 parts of ammonium acetate, 12 parts of modified epoxy resin, 10 parts of aminated carboxymethyl chitosan and 10 parts of oxidized dextran.
The preparation method of the environment-friendly flame-retardant high-strength fiber composite board mainly comprises the following preparation steps:
(1) Mixing the wrinkle layered substance dispersion liquid with absolute ethyl alcohol according to a volume ratio of 1;
(2) Mixing aminated carboxymethyl chitosan and water in a beaker according to a mass ratio of 1:10, adding silicon dioxide which is 1.2 times of the mass of the aminated carboxymethyl chitosan into the beaker, stirring and mixing for 2h, adjusting the pH value of materials in the beaker to 13 by using a sodium hydroxide solution with the concentration of 1mol/L, filtering to obtain a modified silicon dioxide blank, washing the modified silicon dioxide blank with deionized water until the washing solution is neutral, drying for 3h at the temperature of 80 ℃ to obtain modified silicon dioxide, mixing epoxy resin E-51 with phthalic anhydride according to a mass ratio of 5:2, adding modified silicon dioxide which is 0.06 times of the mass of epoxy resin E-51, stirring and mixing for 20min at the temperature of 65 ℃ to obtain an epoxy resin E-51 mixture, coating the epoxy resin E-51 mixture on the wrinkled surface of the modified polyurethane film obtained in the step (1), controlling the using amount of the epoxy resin E-51 mixture to be 4mL/g, keeping the temperature at 180 ℃ for 3h to obtain a modified epoxy resin blank, crushing the modified epoxy resin E-51 mixture, and sieving by using a sieve to obtain modified epoxy resin;
(3) Mixing and soaking wood fibers and water for 24 hours according to a mass ratio of 1;
(4) Weighing the following components in percentage by mass: 70 parts of the pretreated wood fiber obtained in the step (3), 8 parts of calcium oxide, 5 parts of ammonium acetate, 12 parts of the modified epoxy resin obtained in the step (2), 10 parts of aminated carboxymethyl chitosan and 10 parts of oxidized dextran, mixing the pretreated wood fiber obtained in the step (3) and the modified epoxy resin obtained in the step (2) in a stirrer, adding the calcium oxide, the ammonium acetate, the aminated carboxymethyl chitosan and the oxidized dextran into the stirrer, and stirring and mixing to obtain a mixture;
(5) And (3) firstly pressing the mixture obtained in the step (4) for 5min under the conditions of the pressure of 1.5MPa and the temperature of 200 ℃, keeping the pressure, cooling to 80 ℃, pressing for 5min at constant temperature and constant pressure, then pressing for 5min at constant temperature and constant pressure under the conditions of the pressure of 3MPa and the temperature of 200 ℃, keeping the pressure, cooling to 80 ℃, continuing to press for 5min, finally pressing for 5min at constant temperature and constant pressure under the conditions of the pressure of 4.5MPa and the temperature of 200 ℃, cooling to room temperature, discharging, and thus obtaining the environment-friendly flame-retardant high-strength fiber composite board.
Optimally, the preparation method of the wrinkled laminar dispersion liquid in the step (1) comprises the steps of mixing titanium dihydride powder, aluminum powder and graphite powder according to a molar ratio of 3: 1.1; the thickness of the polyurethane film in the step (1) is 0.6mm.
Optimally, the preparation method of the aminated carboxymethyl chitosan in the step (2) and the step (4) comprises the steps of mixing carboxymethyl chitosan with phosphate buffer solution with the pH value of 5.0 according to the mass ratio of 1.
As an optimization, the preparation method of the oxidized dextran in the step (4) comprises the following steps of mixing dextran and deionized water according to a mass ratio of 1:10, mixing, stirring for dissolving, adding 100g/L potassium periodate solution with the mass of 3 times of that of the glucan, reacting for 5 hours at 25 ℃ in a dark place, adding diethylene glycol with the mass of 0.1 time of that of the glucan to obtain an oxidized glucan mixture, dialyzing the oxidized glucan mixture in a dialysis bag with the molecular weight cutoff of 3500 for 72 hours to obtain an oxidized glucan blank, and freeze-drying the oxidized glucan blank to obtain the oxidized glucan.
Example 5
An environment-friendly flame-retardant high-strength fiber composite board mainly comprises the following components in parts by weight: 70 parts of pretreated wood fiber, 8 parts of calcium oxide, 5 parts of ammonium acetate and 12 parts of modified epoxy resin.
The preparation method of the environment-friendly flame-retardant high-strength fiber composite board mainly comprises the following preparation steps:
(1) Mixing the folded laminar dispersion liquid with absolute ethyl alcohol according to a volume ratio of 1;
(2) Mixing aminated carboxymethyl chitosan and water in a beaker according to a mass ratio of 1:10, adding silicon dioxide which is 1.2 times of the mass of aminated carboxymethyl chitosan into the beaker, stirring and mixing for 2h, adjusting the pH value of materials in the beaker to 13 by using a sodium hydroxide solution with the concentration of 1mol/L, filtering to obtain a modified silicon dioxide blank, washing the modified silicon dioxide blank by using deionized water until the washing solution is neutral, drying for 3h at the temperature of 80 ℃ to obtain modified silicon dioxide, mixing epoxy resin E-51 with phthalic anhydride according to a mass ratio of 5:2, adding modified silicon dioxide which is 0.06 times of the mass of epoxy resin E-51, stirring and mixing for 20min at the temperature of 65 ℃ to obtain an epoxy resin E-51 mixture, vacuumizing the epoxy resin E-51 mixture for 15min at the temperature of 80 ℃, coating the epoxy resin E-51 mixture on the wrinkled surface of the modified film obtained in the step (1), controlling the use amount of the epoxy resin E-51 mixture to be 4mL/g, heating to the constant temperature of 80 ℃ for 15min, heating to 2 ℃/5 h, heating to obtain a modified epoxy resin wrinkled surface, heating to obtain a temperature-keeping blank, and heating to obtain a temperature-modified epoxy resin, and heating to 2 ℃/3 h, and heating to obtain a temperature-modified polyurethane wrinkled surface after heating to obtain a temperature-modified epoxy resin blank, wherein the epoxy resin blank, the epoxy resin is heated to obtain a temperature-modified polyurethane wrinkled rate of the epoxy resin, and the epoxy resin after heating rate of 2 ℃/3 h;
(3) Mixing and soaking wood fibers and water for 24 hours according to a mass ratio of 1;
(4) Weighing the following components in sequence according to mass fraction: 70 parts of the pretreated wood fiber obtained in the step (3), 8 parts of calcium oxide, 5 parts of ammonium acetate and 12 parts of the modified epoxy resin obtained in the step (2), mixing the pretreated wood fiber obtained in the step (3) and the modified epoxy resin obtained in the step (2) in a stirrer, adding the calcium oxide and the ammonium acetate into the stirrer, and stirring and mixing to obtain a mixture;
(5) And (5) pressing the mixture obtained in the step (4) for 5min under the conditions of pressure of 1.5MPa and temperature of 200 ℃, maintaining the pressure, cooling to 80 ℃, pressing for 5min at constant temperature and constant pressure, then pressing for 5min at constant temperature and constant pressure under the conditions of pressure of 3MPa and temperature of 200 ℃, maintaining the pressure, cooling to 80 ℃, continuing to press for 5min, finally pressing for 5min at constant temperature and constant pressure under the conditions of pressure of 4.5MPa and temperature of 200 ℃, cooling to room temperature, and discharging to obtain the environment-friendly flame-retardant high-strength fiber composite board.
Optimally, the preparation method of the wrinkled laminar dispersion liquid in the step (1) comprises the steps of mixing titanium dihydride powder, aluminum powder and graphite powder according to a molar ratio of 3: 1.1; the thickness of the polyurethane film in the step (1) is 0.6mm.
Optimally, the preparation method of the aminated carboxymethyl chitosan in the step (2) comprises the steps of mixing carboxymethyl chitosan with phosphate buffer solution with pH of 5.0 according to a mass ratio of 1.
Comparative example
An environment-friendly flame-retardant high-strength fiber composite board mainly comprises the following components in parts by weight: 70 parts of pretreated wood fiber, 8 parts of calcium oxide, 5 parts of ammonium acetate and 12 parts of modified epoxy resin.
The preparation method of the environment-friendly flame-retardant high-strength fiber composite board mainly comprises the following preparation steps:
(1) Mixing the folded laminar dispersion liquid with absolute ethyl alcohol according to a volume ratio of 1;
(2) Mixing epoxy resin E-51 with phthalic anhydride according to a mass ratio of 5 to 2, adding silicon dioxide which is 0.06 times of the mass of the epoxy resin E-51, stirring and mixing for 20min at 65 ℃ to obtain an epoxy resin E-51 mixture, coating the epoxy resin E-51 mixture on the wrinkled surface of the modified polyurethane film obtained in the step (1), controlling the using amount of the epoxy resin E-51 mixture to be 4mL/g, keeping the temperature at 180 ℃ for 3h to obtain a modified epoxy resin blank, crushing the modified epoxy resin blank, and sieving with a 5-mesh sieve to obtain the modified epoxy resin;
(3) Mixing and soaking wood fibers and water for 24 hours according to a mass ratio of 1;
(4) Weighing the following components in sequence according to mass fraction: 70 parts of the pretreated wood fiber obtained in the step (3), 8 parts of calcium oxide, 5 parts of ammonium acetate and 12 parts of the modified epoxy resin obtained in the step (2), mixing the pretreated wood fiber obtained in the step (3) and the modified epoxy resin obtained in the step (2) in a stirring machine, adding the calcium oxide and the ammonium acetate into the stirring machine, and stirring and mixing to obtain a mixture;
(5) And (5) pressing the mixture obtained in the step (4) for 5min under the conditions of pressure of 1.5MPa and temperature of 200 ℃, maintaining the pressure, cooling to 80 ℃, pressing for 5min at constant temperature and constant pressure, then pressing for 5min at constant temperature and constant pressure under the conditions of pressure of 3MPa and temperature of 200 ℃, maintaining the pressure, cooling to 80 ℃, continuing to press for 5min, finally pressing for 5min at constant temperature and constant pressure under the conditions of pressure of 4.5MPa and temperature of 200 ℃, cooling to room temperature, and discharging to obtain the environment-friendly flame-retardant high-strength fiber composite board.
As optimization, the preparation method of the silicon dioxide dispersion liquid in the step (1) comprises the steps of mixing nano silicon dioxide and water according to the mass ratio of 1; the thickness of the polyurethane film in the step (1) is 0.6mm.
Effects of the invention
Table 1 below shows the performance analysis results of the environment-friendly flame-retardant high-strength fiber composite panels using examples 1 to 3 of the present invention and a comparative example.
TABLE 1
| Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Comparative example | |
| Static bending strength (MPa) | 24.3 | 20.8 | 19.2 | 18.6 | 17.2 | 14.2 |
| Limiting oxygen index (%) | 29.6 | 28.1 | 26.2 | 25.6 | 28.2 | 24.6 |
Compared with the experimental data of the example 1 and the comparative example 1 in the table 1, the mechanical property and the flame retardant property of the product can be effectively improved when the modified epoxy resin, the aminated carboxymethyl chitosan and the oxidized dextran are added during the preparation of the environment-friendly flame retardant high-strength fiber composite board; from the experimental data of example 1 and example 2, when the modified epoxy resin is prepared, when the aminated carboxymethyl chitosan modified silica is not added, the internal bonding force of the product is reduced, and the reaction rate of the aminated carboxymethyl chitosan and the oxidized dextran is reduced, thereby affecting the mechanical properties of the product, from the experimental data of example 1 and example 3, it can be found that when the surface coated with the shape memory material in the modified epoxy resin is not wrinkled during the preparation of the environment-friendly flame-retardant high-strength fiber composite board, the bonding force between fibers in the product is reduced, and the carbonaceous material and the silica are not well dispersed, thereby affecting the flame retardant properties and the mechanical properties of the product, from the experimental data of example 1 and example 4, when the shape memory material is not contained in the modified epoxy resin added during the preparation of the environment-friendly flame-retardant high-strength fiber composite board, the strength and the mechanical properties of the product can also be affected.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Claims (1)
1. The environment-friendly flame-retardant high-strength fiber composite board is characterized in that: the adhesive mainly comprises the following components in parts by weight: 70 parts of pretreated wood fiber, 8 parts of calcium oxide, 5 parts of ammonium acetate, 12 parts of modified epoxy resin, 10 parts of aminated carboxymethyl chitosan and 10 parts of oxidized dextran;
the preparation method of the environment-friendly flame-retardant high-strength fiber composite board mainly comprises the following preparation steps:
(1) Mixing the folded laminar dispersion liquid with absolute ethyl alcohol according to a volume ratio of 1;
(2) Mixing aminated carboxymethyl chitosan and water in a beaker according to a mass ratio of 1:10, adding silicon dioxide which is 1.2 times of the mass of aminated carboxymethyl chitosan into the beaker, stirring and mixing for 2h, adjusting the pH value of materials in the beaker to 13 by using a sodium hydroxide solution with the concentration of 1mol/L, filtering to obtain a modified silicon dioxide blank, washing the modified silicon dioxide blank by using deionized water until the washing solution is neutral, drying for 3h at the temperature of 80 ℃ to obtain modified silicon dioxide, mixing epoxy resin E-51 with phthalic anhydride according to a mass ratio of 5:2, adding modified silicon dioxide which is 0.06 times of the mass of epoxy resin E-51, stirring and mixing for 20min at the temperature of 65 ℃ to obtain an epoxy resin E-51 mixture, vacuumizing the epoxy resin E-51 mixture for 15min at the temperature of 80 ℃, coating the epoxy resin E-51 mixture on the wrinkled surface of the modified film obtained in the step (1), controlling the use amount of the epoxy resin E-51 mixture to be 4mL/g, heating to the constant temperature of 80 ℃ for 15min, heating to 2 ℃/5 h, heating to obtain a modified epoxy resin wrinkled surface, heating to obtain a temperature-keeping blank, and heating to obtain a temperature-modified epoxy resin, and heating to 2 ℃/3 h, and heating to obtain a temperature-modified polyurethane wrinkled surface after heating to obtain a temperature-modified epoxy resin blank, wherein the epoxy resin blank, the epoxy resin is heated to obtain a temperature-modified polyurethane wrinkled rate of the epoxy resin, and the epoxy resin after heating rate of 2 ℃/3 h;
(3) Mixing and soaking wood fibers and water for 24 hours according to a mass ratio of 1;
(4) Weighing the following components in percentage by mass: 70 parts of the pretreated wood fiber obtained in the step (3), 8 parts of calcium oxide, 5 parts of ammonium acetate, 12 parts of the modified epoxy resin obtained in the step (2), 10 parts of aminated carboxymethyl chitosan and 10 parts of oxidized dextran, mixing the pretreated wood fiber obtained in the step (3) and the modified epoxy resin obtained in the step (2) in a stirrer, adding the calcium oxide, the ammonium acetate, the aminated carboxymethyl chitosan and the oxidized dextran into the stirrer, and stirring and mixing to obtain a mixture;
(5) Pressing the mixture obtained in the step (4) for 5min under the conditions of pressure of 1.5MPa and temperature of 200 ℃, keeping the pressure, cooling to 80 ℃, pressing for 5min at constant temperature and constant pressure, then pressing for 5min at constant temperature and constant pressure under the conditions of pressure of 3MPa and temperature of 200 ℃, keeping the pressure, cooling to 80 ℃, continuing to press for 5min, finally, pressing for 5min at constant temperature and constant pressure under the conditions of pressure of 4.5MPa and temperature of 200 ℃, cooling to room temperature, discharging, and obtaining the environment-friendly flame-retardant high-strength fiber composite board;
mixing titanium dihydride powder, aluminum powder and graphite powder according to a molar ratio of 3, performing ball milling to obtain mixed powder, placing the mixed powder in an argon atmosphere, sintering for 2 hours at the temperature of 1400 ℃ to obtain a layered product, mixing hydrochloric acid and fluorine according to a mass ratio of 2; the thickness of the polyurethane film in the step (1) is 0.6mm;
mixing carboxymethyl chitosan with phosphate buffer solution with pH of 5.0 according to a mass ratio of 1;
the preparation method of the oxidized glucan in the step (4) comprises the following steps of mixing glucan and deionized water according to the mass ratio of 1:10, mixing, stirring for dissolving, adding 100g/L potassium periodate solution with the mass of 3 times of that of the glucan, reacting for 5 hours at 25 ℃ in a dark place, adding diethylene glycol with the mass of 0.1 time of that of the glucan to obtain an oxidized glucan mixture, dialyzing the oxidized glucan mixture in a dialysis bag with the molecular weight cutoff of 3500 for 72 hours to obtain an oxidized glucan blank, and freeze-drying the oxidized glucan blank to obtain the oxidized glucan.
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