CN108943245B - Preparation method of multifunctional carbonized wood - Google Patents
Preparation method of multifunctional carbonized wood Download PDFInfo
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- CN108943245B CN108943245B CN201810989846.0A CN201810989846A CN108943245B CN 108943245 B CN108943245 B CN 108943245B CN 201810989846 A CN201810989846 A CN 201810989846A CN 108943245 B CN108943245 B CN 108943245B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B27—WORKING OR PRESERVING WOOD OR SIMILAR MATERIAL; NAILING OR STAPLING MACHINES IN GENERAL
- B27M—WORKING OF WOOD NOT PROVIDED FOR IN SUBCLASSES B27B - B27L; MANUFACTURE OF SPECIFIC WOODEN ARTICLES
- B27M1/00—Working of wood not provided for in subclasses B27B - B27L, e.g. by stretching
- B27M1/06—Working of wood not provided for in subclasses B27B - B27L, e.g. by stretching by burning or charring, e.g. cutting with hot wire
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B27—WORKING OR PRESERVING WOOD OR SIMILAR MATERIAL; NAILING OR STAPLING MACHINES IN GENERAL
- B27K—PROCESSES, APPARATUS OR SELECTION OF SUBSTANCES FOR IMPREGNATING, STAINING, DYEING, BLEACHING OF WOOD OR SIMILAR MATERIALS, OR TREATING OF WOOD OR SIMILAR MATERIALS WITH PERMEANT LIQUIDS, NOT OTHERWISE PROVIDED FOR; CHEMICAL OR PHYSICAL TREATMENT OF CORK, CANE, REED, STRAW OR SIMILAR MATERIALS
- B27K3/00—Impregnating wood, e.g. impregnation pretreatment, for example puncturing; Wood impregnation aids not directly involved in the impregnation process
- B27K3/02—Processes; Apparatus
- B27K3/08—Impregnating by pressure, e.g. vacuum impregnation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B27—WORKING OR PRESERVING WOOD OR SIMILAR MATERIAL; NAILING OR STAPLING MACHINES IN GENERAL
- B27K—PROCESSES, APPARATUS OR SELECTION OF SUBSTANCES FOR IMPREGNATING, STAINING, DYEING, BLEACHING OF WOOD OR SIMILAR MATERIALS, OR TREATING OF WOOD OR SIMILAR MATERIALS WITH PERMEANT LIQUIDS, NOT OTHERWISE PROVIDED FOR; CHEMICAL OR PHYSICAL TREATMENT OF CORK, CANE, REED, STRAW OR SIMILAR MATERIALS
- B27K5/00—Treating of wood not provided for in groups B27K1/00, B27K3/00
- B27K5/007—Treating of wood not provided for in groups B27K1/00, B27K3/00 using pressure
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B27—WORKING OR PRESERVING WOOD OR SIMILAR MATERIAL; NAILING OR STAPLING MACHINES IN GENERAL
- B27K—PROCESSES, APPARATUS OR SELECTION OF SUBSTANCES FOR IMPREGNATING, STAINING, DYEING, BLEACHING OF WOOD OR SIMILAR MATERIALS, OR TREATING OF WOOD OR SIMILAR MATERIALS WITH PERMEANT LIQUIDS, NOT OTHERWISE PROVIDED FOR; CHEMICAL OR PHYSICAL TREATMENT OF CORK, CANE, REED, STRAW OR SIMILAR MATERIALS
- B27K5/00—Treating of wood not provided for in groups B27K1/00, B27K3/00
- B27K5/06—Softening or hardening of wood
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- Wood Science & Technology (AREA)
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- Chemical And Physical Treatments For Wood And The Like (AREA)
Abstract
A preparation method of multifunctional carbonized wood, which relates to a preparation method of carbonized wood. The invention aims to solve the problem that the existing wood modification method can not synchronously improve the mechanical strength, impact toughness and waterproof performance of wood and endow the wood with functions of sterilization, flame retardance, magnetism and the like. The method comprises the following steps: 1. wood softening pretreatment; 2. performing super-hydrophobic treatment on the softened wood composite inorganic nano material; 3. compressing and densifying the wood; 4. and (3) carrying out high-temperature carbonization treatment on the wood. The wood modified by the method has a micro-nano hierarchical microstructure given by inorganic nano materials and abrasive paper, the inorganic nano materials are arranged inside and on the surface of the wood, the wood substrate is further covered by hydrophobic substances, the microstructure of the wood is similar to that of lotus leaves, the porous structure of the wood is compressed and compacted, the wood has a super-hydrophobic function, and the tensile strength, the compressive strength, the impact toughness, the hardness, the wear resistance, the elastic modulus and the static bending strength are obviously improved. The invention is used in the field of wood modification.
Description
Technical Field
The invention relates to a preparation method of carbonized wood.
Background
The wood is easy to absorb water, expand and deform due to complex and unique components (mainly cellulose, hemicellulose and lignin), is easy to corrode, decay and degrade by mould, is easy to be degraded by thermal combustion and the like; the density and strength of the fast-growing wood species (such as poplar, fir, birch and the like) are low due to loose and porous structure, and are particularly so. In order to improve the strength of wood, prolong the service life of wood (improve the durability of wood such as water resistance, corrosion resistance, flame retardance and the like), and even endow wood with some unique functions such as magnetism and the like, people adopt various methods to modify wood, and in summary, the method mainly comprises the following steps: 1. vinyl monomers are utilized to form polymer filled wood through free radical polymerization in a wood cellular cavity structure, or prepolymers (phenolic resin, melamine resin and the like) are utilized to form polymer filled wood through polycondensation in the wood cellular cavity structure, so that the wood density is increased, the mechanical property is improved, and meanwhile, the durability (dimensional stability and corrosion resistance) is partially improved, but the method can cause the brittleness and the impact toughness of the wood to be increased; 2. the whole or the surface of the wood is subjected to hydrothermal softening, and then the wood entity or the surface of the wood is compressed along the direction vertical to the axial direction of the wood, so that the whole or the surface of the wood is compact, and the aim of improving the strength of the wood by increasing the compactness of the compressed wood is achieved, but the compressed and compacted wood prepared by the method cannot resist water, and can rebound in size when encountering water, although people fix the compressed and compacted wood by adopting polymers such as phenolic resin and the like can prevent the size of the wood from rebounding when encountering water to a certain extent, the impact toughness of the compressed and compacted wood is greatly reduced, and the brittleness is increased; 3. the wood is subjected to high-temperature (180-220 ℃) heat treatment, so that hemicellulose in the wood is degraded to a certain extent, and the environment-friendly carbonized wood with good size stability and certain corrosion resistance is obtained and is deeply favored by the market, but the brittleness of the wood is increased, and the mechanical property is reduced; 4. the nanometer technology is utilized to generate nanometer inorganic bodies (such as silicon dioxide, titanium dioxide, zinc oxide, silver, ferroferric oxide and the like) in situ in the wood or directly fill the nanometer inorganic bodies, so that the wood is endowed with super waterproof, even sterilization, flame retardant, electromagnetic shielding and other functions, and the waterproof performance of the wood is fundamentally improved, but the method is difficult to effectively improve the mechanical strength of the wood. In a word, the current treatment method cannot find a balance point between the improvement of the mechanical strength of the wood and the permanent water resistance of the wood, namely, the strength and the water resistance of the wood cannot be synchronously improved, and other functional characteristics cannot be synchronously endowed.
In recent years, with the social development and the improvement of the living standard of people, the role of wood in human life is more and more important; meanwhile, the contradiction between the demand of wood and the shortage of wood supply is more and more sharp, so that the strength, the waterproof performance, the sterilization and corrosion resistance, the flame retardant performance and the like of wood (particularly wood of low-quality fast-growing tree species) are synchronously and obviously improved by improving the wood through a proper technology, and even the wood has a unique magnetic function, is expected to greatly improve the added value of the wood, broaden the application range of the wood, prolong the service life of the wood and relieve the dilemma of the shortage of wood supply.
Disclosure of Invention
The invention provides a preparation method of multifunctional carbonized wood, aiming at solving the problems that the existing wood modification method can not synchronously improve the mechanical strength, impact toughness and waterproof performance of wood and endow the wood with functions of sterilization, flame retardation, magnetism and the like.
The preparation method of the multifunctional carbonized wood comprises the following steps:
1. wood softening pretreatment:
soaking wood in distilled water, heating to 100 deg.C, and steaming for 2 hr to obtain softened wood;
or putting the wood into NaOH aqueous solution with the mass concentration of 1.5-3 wt%, heating for 2-4 h at 90 ℃ to remove most hemicellulose, and then washing the wood to be neutral by distilled water at room temperature to obtain the softened wood.
Or steam with the temperature of 120 ℃ is used for steaming the surface of the wood for 2 hours, and the softened wood is obtained.
2. Super-hydrophobization treatment of the softened wood composite inorganic nano material:
(1) adding an inorganic nano material with the diameter or thickness of 1-100nm into toluene, adding polydimethylsiloxane, then performing ultrasonic dispersion for 1-1.5 h under the power of 500-550 Hz, and then mechanically stirring for 70-74 h at the room temperature at the speed of 1000-1200 rpm; centrifuging at 6000-7000 rpm for 15-30 min, washing with dichloromethane and acetone for 3-5 times, centrifuging at 6000-7000 rpm for 15-30 min, and drying at 90-110 deg.C for 22-26 h; wherein the volume ratio of the mass of the inorganic nano material to the toluene is 1g: (90-110) mL, wherein the mass ratio of the inorganic nano material to the polydimethylsiloxane is 1 (0.5-0.7);
(2) adding the inorganic nano material treated in the step one into absolute ethyl alcohol, then dropwise adding fluorosilane as a hydrophobic substance, mechanically stirring at the speed of 1000-1200 rpm for 1-1.5 h, then ultrasonically dispersing for 1-1.5 h under the power of 500-550 Hz, and finally stirring at the temperature of 60-65 ℃ for 30-40 min to obtain liquid;
(3) and (3) putting the wood into the liquid obtained in the step (2), pressurizing for 30-40 min under the pressure of 0.8-0.9 MPa, recovering to normal pressure, and taking out the wood to finish the super-hydrophobization treatment of the softened wood composite inorganic nano material.
3. Wood compression and densification treatment:
completely covering the upper and lower surfaces of the wood treated in the second step by using two 120-mesh abrasive paper to enable the rough surface of the abrasive paper to be in contact with the wood, then placing the wood with the abrasive paper in a hot press, and compressing the wood to 20% -25% of the original thickness under the conditions of room temperature and 5-10 MPa; and then gradually heating: heating to 60-80 ℃ and keeping the pressure for 8-10h, then continuously heating to 100-120 ℃ and keeping the pressure for 24-48h, then cooling the hot press to room temperature at the speed of 20 ℃/h while keeping the pressure, then recovering to normal pressure and removing the abrasive paper to finish the wood compression and densification treatment, wherein the thickness of the wood is compressed to 20% -25% of the original thickness.
4. High-temperature carbonization treatment of wood:
putting the wood treated in the third step into a high-temperature carbonization box, heating to 130-150 ℃ at the speed of 5-10 ℃/h, preserving heat for 2-3h, then continuously heating to 180-200 ℃ at the speed of 5-10 ℃/h, and preserving heat for 24-48h; or continuously placing the mixture into a hot press, heating to 180-200 ℃ at the speed of 5-10 ℃/h under the pressure of 5-10MPa in the third step, and preserving heat for 24-48h.
Then, gradually cooling to 150 ℃ at the speed of 3-5 ℃/h, preserving heat for 2-3h, and spraying steam on the wood every 1h in the heat preservation stage for 10min; then, gradually cooling to 120 ℃ at the speed of 3-5 ℃/h, preserving heat for 2-3h, and spraying water vapor on the wood every 1h in the heat preservation stage for 10min; then the temperature is gradually reduced to 100 ℃ at the speed of 5-10 ℃/h and is kept for 2-3h; and finally, cooling to room temperature at the speed of 10-20 ℃/h to obtain the multifunctional carbonized wood.
Further, in the second step (1), the inorganic nano-material is nano-silica, nano-titanium dioxide, nano-silver, nano-zinc oxide, nano-ferroferric oxide, nano-calcium carbonate, two-dimensional nano-clay, two-dimensional nano-boron nitride, two-dimensional graphene or two-dimensional graphene oxide, or a composite of two or more of the nano-materials in any proportion, but the inorganic nano-material is not limited to these nano-materials
Furthermore, the mass ratio of the inorganic nano material to the absolute ethyl alcohol in the step two (2) is 1 (29-31), and the mass ratio of the inorganic nano material to the fluorosilane is 1 (0.2-0.4).
Further, in the second step (3), the fluorosilane is one or a mixture of more of heptadecafluorotrimethoxysilane, heptadecafluorotriethoxysilane, tridecafluorosilyltrimethoxysilane and tridecafluorosilyltriethoxysilane in any ratio.
The invention has the beneficial effects that:
the invention provides the preparation method of the multifunctional carbonized wood, which is simple to operate, environment-friendly and low in cost, and integrates the functions of super water resistance, high strength, even partial sterilization, flame retardance, magnetism and the like.
In order to increase the strength of the wood, the invention applies hot pressing treatment to the surface of the wood, so that the surface of the wood has no micron-scale coarse structure, and therefore, while compounding the inorganic nano material, 120-mesh abrasive paper is covered to copy the micron-scale coarse structure of the abrasive paper to the surface of the wood during hot pressing, so that the wood has a micron-scale coarse result, and the wood can be endowed with a super-hydrophobic function by combining the nano-scale size structure of the inorganic nano material, and simultaneously has high strength and good wear resistance. The purpose of the hot pressing of coated abrasive paper of the present invention is to increase the roughness (unevenness) of the wood surface, thereby imparting super-hydrophobic characteristics.
The softening treatment in the first step is convenient for (1) the wood is more easily compressed and densified to avoid that the cell walls are crushed and broken in the compression process to negatively influence the mechanical strength, (2) a large amount of hemicellulose can be removed when alkaline water liquid is softened at high temperature, so that the water absorption and resilience phenomenon after the wood is compressed is effectively avoided, and (3) a large amount of hemicellulose is removed by softening, so that enough nano space is provided for storing subsequent nano functional particles, thereby providing conditions for enriching the functionality of the wood, facilitating the subsequent compression process, and firmly sealing the nano functional particles in the wood by compression, so that the functionality is longer; adding inorganic nano materials into the wood cell cavities, endowing the wood with a nano-scale rough structure so as to construct a super-hydrophobic surface structure, and endowing the wood with unique functions of sterilization, flame retardance, even magnetism and the like; the third step of compression and densification can increase the density of the wood and enable the wood cells to be compressed to be flat, the densified layered structure can endow the wood with high strength, high hardness and toughness, and the surface of the wood can be endowed with micron-sized protrusions by the sand paper loaded on the surface, so that the construction of a super-hydrophobic function is facilitated; and step four, further removing partial hemicellulose in the wood by high-temperature carbonization treatment, so that the dimensional stability of the wood is improved, and the corrosion resistance and the thermal stability are partially improved. In addition, the compression and carbonization combined treatment of the wood can firmly limit the nano material in the wood, thereby improving the problem of water loss of the nano material in the wood.
The inorganic nano material is coated by polydimethylsiloxane, so that the inorganic nano material has certain hydrophobicity; then, the fluorosilane is hydrolyzed in ethanol to form fluorosilane with hydroxyl, and then hydrolyzed and condensed with the inorganic nano material coated with a certain amount of polydimethylsiloxane to form the fluorosilanized nano material, so that the nano material has high hydrophobicity; then, after the inorganic nano material, the hydrolyzed fluorosilane and the ethanol are soaked into the wood, the fluorosilane can further perform condensation reaction with the wood through hydroxyl, so that the surfaces of the wood components are hydrophobized by the fluorosilane, and the wood becomes super-hydrophobic under the action of the micro-nano hierarchical structure and the hydrophobic substance; it combines the double hydrophobic functions of dimethyl silicone polymer and fluorosilane, so that it possesses excellent super-hydrophobic function.
The wood modified by the method has a micro-nano hierarchical microstructure given by inorganic nano materials and abrasive paper, the inorganic nano materials are arranged inside and on the surface of the wood, the wood substrate is further covered by fluorine-containing hydrophobic substances, the microstructure of the wood is similar to that of lotus leaves, the porous structure of the wood is compressed and compacted, and the hydrophobic angle of each surface of the prepared wood is more than 150 degrees, namely the modified wood has a super-hydrophobic function; the static water contact angle of the radial section of the wood after being rubbed for 20 times by a weight of 100g loaded by 240-mesh sand paper is still more than 150 degrees, the rolling angle is less than 10 degrees, and the water absorption capacity of the wood after being continuously soaked in water for 10 days is less than 5 percent.
The tensile strength of the wood modified by the method can reach 360-399 MPa, the compressive strength (end face) can reach 170-210 MPa, and the impact toughness (tangent plane) can reach 135-147 KJ/m 2 The hardness can reach 8500-10800N, the wear resistance can reach 0.8-1.0, the elastic modulus can reach 14000-18000 MPa, the static bending strength can reach 190-230 MPa, the mass loss rate after 12 weeks of corrosion is 90% -92%, and the peak value of the heat release rate measured by a cone calorimeter is 460-575 kW/m 2 。
The tensile strength, the compressive strength, the impact toughness, the hardness, the wear resistance, the elastic modulus and the static bending strength of the modified wood are respectively improved by 5 to 7 times, 2.5 to 4 times, 2 to 3 times, 3 to 5 times, 2.4 to 3.6 times, 1.8 to 2.7 times and 2.2 to 3.3 times compared with the untreated wood, the corrosion resistance is improved, the flame retardant property is obviously improved, and even the carbonized wood treated by the nano ferroferric oxide has paramagnetism.
The wood obtained by the treatment method is expected to be used in the fields of building structural materials, sports equipment materials and transportation materials with higher requirements on material strength indoors and outdoors.
Drawings
FIG. 1 is an SEM topography of a cross section of a multifunctional carbonized wood based on nano-silica in example 1;
FIG. 2 is an SEM topography of a longitudinal section of the nano-silica based multifunctional carbonized wood in example 1;
FIG. 3 is the static water contact angle of a diametric section of wood prepared in example 1;
FIG. 4 is an SEM topography of a cross section of the multifunctional carbonized wood based on nano ferroferric oxide in example 2;
FIG. 5 is an SEM topography of a longitudinal section of the multifunctional carbonized wood based on nano ferroferric oxide in example 2;
FIG. 6 is a radial cut section of the wood prepared in example 2 for the hydrophobic angle;
FIG. 7 is an SEM topography of a cross section of the nano-silver based multifunctional carbonized wood in example 3;
FIG. 8 is an SEM topography of a longitudinal section of the multifunctional carbonized wood based on nano-silver in example 3;
FIG. 9 is the wood diametral section hydrophobic angle prepared in example 3;
FIG. 10 is an SEM topography of the boron nitride in the multifunctional carbonized wood cell cavity based on two-dimensional layered nano boron nitride in example 4;
FIG. 11 is an SEM topography of a cross section of the multifunctional carbonized wood based on two-dimensional layered nano boron nitride in example 4;
FIG. 12 is the wood diametral section hydrophobic angle prepared in example 4;
fig. 13 is an EDX (energy dispersive analysis) of elements corresponding to the cross section of the multifunctional carbonized wood based on two-dimensional layered nano boron nitride in example 4.
Detailed Description
The technical solution of the present invention is not limited to the following specific embodiments, but includes any combination of the specific embodiments.
The first embodiment is as follows: the preparation method of the multifunctional carbonized wood of the embodiment comprises the following steps:
1. wood softening pretreatment:
putting wood into NaOH aqueous solution with the mass concentration of 1.5-3 wt%, heating for 2-4 h at 90 ℃ to remove most hemicellulose, and then washing the wood to be neutral by distilled water at room temperature to obtain softened wood.
2. Super-hydrophobization treatment of the softened wood composite inorganic nano material:
(1) adding inorganic nano material with the diameter or thickness of 1-100nm into toluene, adding polydimethylsiloxane, then carrying out ultrasonic dispersion, and mechanically stirring at room temperature for 70-74 h; centrifuging for 15-30 min, repeatedly washing with dichloromethane and acetone for 3-5 times, centrifuging for 15-30 min, and drying for 22-26 h; wherein the volume ratio of the mass of the inorganic nano material to the toluene is 1g: (90-110) mL, wherein the mass ratio of the inorganic nano material to the polydimethylsiloxane is 1 (0.5-0.7);
(2) adding the inorganic nano material treated in the step one into absolute ethyl alcohol, then dropwise adding fluorosilane as a hydrophobic substance, then mechanically stirring for 1-1.5 h, then performing ultrasonic dispersion, and finally stirring at 60-65 ℃ for 30-40 min to obtain liquid;
(3) putting wood into the liquid obtained in the step (2), pressurizing for 30-40 min under the pressure of 0.8-0.9 MPa, recovering to normal pressure, and taking out the wood to finish the super-hydrophobization treatment of the softened wood composite inorganic nano material;
3. wood compression and densification treatment:
completely covering the upper and lower surfaces (radial sections) of the wood treated in the second step by using two 120-mesh abrasive paper to enable the rough surface of the abrasive paper to be in contact with the wood, then placing the wood with the abrasive paper in a hot press, and compressing the wood to 20-25% of the original thickness under the conditions of room temperature and 5-10 MPa; and then gradually heating: firstly heating to 60-80 ℃ and keeping the pressure for 8-10h, then continuously heating to 100-120 ℃ and keeping the pressure for 24-48h, then cooling the hot press to room temperature at the speed of 20 ℃/h under the condition of keeping the pressure, then recovering to normal pressure and removing abrasive paper to finish the compression and densification treatment of the wood;
4. high-temperature carbonization treatment of wood:
putting the wood treated in the third step into a high-temperature carbonization box, heating to 130-150 ℃ at the speed of 5-10 ℃/h, preserving heat for 2-3h, then continuously heating to 180-200 ℃ at the speed of 5-10 ℃/h, and preserving heat for 24-48h; or continuously placing the mixture in a hot press, heating the mixture to 180-200 ℃ at the speed of 5-10 ℃/h under the pressure of 5-10MPa in the third step, and preserving the heat for 24-48h;
then, gradually cooling to 150 ℃ at the speed of 3-5 ℃/h, preserving heat for 2-3h, and spraying steam on the wood every 1h for 10min in the heat preservation stage; then, the temperature is gradually reduced to 120 ℃ at the speed of 3-5 ℃/h and is kept for 2-3h, and steam is sprayed on the wood every 1h in the heat-preservation stage for 10min; then the temperature is gradually reduced to 100 ℃ at the speed of 5-10 ℃/h and is kept for 2-3h; finally, cooling to room temperature at the speed of 10-20 ℃/h to obtain the multifunctional carbonized wood.
The second embodiment is as follows: the first difference between the present embodiment and the specific embodiment is: the method for softening the wood in the first step is a cooking method, an alkali treatment method or a steaming method. The rest is the same as the first embodiment.
The third concrete implementation mode: the second difference between this embodiment and the second embodiment is that: the cooking method comprises soaking wood in distilled water, heating to 100 deg.C, and cooking for 2 hr to obtain softened wood. The rest is the same as the second embodiment.
The fourth concrete implementation mode is as follows: the second embodiment is different from the first embodiment in that: the alkali treatment method comprises the steps of putting wood into a NaOH aqueous solution with the mass concentration of 2%, heating for 2 hours at 90 ℃ to remove most hemicellulose, and then washing the wood to be neutral by distilled water at room temperature to obtain softened wood. The rest is the same as the second embodiment.
The fifth concrete implementation mode is as follows: the second embodiment is different from the first embodiment in that: the steaming method is to steam the surface of the wood for 2 hours by using water vapor with the temperature of 120 ℃ to obtain the softened wood. The rest is the same as the second embodiment.
The sixth specific implementation mode is as follows: the first difference between the present embodiment and the specific embodiment is: and in the second step (1), the inorganic nano material is nano silicon dioxide, nano titanium dioxide, nano silver, nano zinc oxide, nano ferroferric oxide, nano calcium carbonate, two-dimensional nano clay, two-dimensional nano boron nitride, two-dimensional graphene or two-dimensional graphene oxide. The rest is the same as the first embodiment.
The seventh embodiment: the first difference between the present embodiment and the specific embodiment is: the power of ultrasonic dispersion in the step two (1) is 500-550 Hz, and the time of ultrasonic dispersion is 1-1.5 h. The rest is the same as the first embodiment.
The specific implementation mode eight: the first difference between the present embodiment and the specific embodiment is: the speed of mechanical stirring in the step two (1) is 1000-1200 rpm. The rest is the same as the first embodiment.
The specific implementation method nine: the first difference between the present embodiment and the specific embodiment is: the rotating speed of the centrifugation in the step two (1) is 6000 to 7000rpm. The rest is the same as the first embodiment.
The specific implementation mode is ten: the first difference between the present embodiment and the specific embodiment is: the drying temperature in the second step (1) is 90-110 ℃. The rest is the same as the first embodiment.
The concrete implementation mode eleven: the first difference between the present embodiment and the specific embodiment is: in the second step (2), the mass ratio of the inorganic nano material to the absolute ethyl alcohol is 1 (29-31), and the mass ratio of the inorganic nano material to the fluorosilane is 1 (0.2-0.4). The rest is the same as the first embodiment.
The detailed implementation mode is twelve: the first difference between the present embodiment and the specific embodiment is: the speed of mechanical stirring in the second step (2) is 1000-1200 rpm. The rest is the same as the first embodiment.
The specific implementation mode is thirteen: the first difference between the present embodiment and the specific embodiment is: the power of ultrasonic dispersion in the step two (2) is 500-550 Hz, and the time of ultrasonic dispersion is 1-1.5 h. The rest is the same as the first embodiment.
The specific implementation mode is fourteen: the first difference between the present embodiment and the specific embodiment is: in the step two (3), the fluorosilane is one or a mixture of a plurality of heptadecafluorotrimethoxysilane, heptadecafluorotriethoxysilane, tridecafluorosilyltrimethoxysilane and tridecafluorosilyltriethoxysilane according to any ratio. The rest is the same as the first embodiment.
The following examples are given to illustrate the present invention, and the following examples are carried out on the premise of the technical solution of the present invention, and give detailed embodiments and specific procedures, but the scope of the present invention is not limited to the following examples.
Example 1: the preparation method of the multifunctional carbonized wood comprises the following steps:
1. wood softening pretreatment:
soaking basswood into distilled water, heating to 100 ℃, and stewing the wood for 2h to obtain softened wood;
2. super-hydrophobization treatment of the softened wood composite inorganic nano material:
(1) adding 1g of inorganic nano silicon dioxide with the mass of 100nm into 100ml of toluene, adding 0.6g of polydimethylsiloxane, then performing ultrasonic dispersion for 1h under the power of 500Hz, and mechanically stirring for 72h at the speed of 1000rpm at room temperature; then, the mixture was centrifuged at 6000rpm for 15min, and repeatedly washed with dichloromethane and acetone 3 times in succession, and after centrifugation at 6000rpm for 15min, the mixture was dried at 100 ℃ for 24 hours.
(2) Adding the inorganic nano material obtained in the step one into 30g of absolute ethyl alcohol, then dropwise adding 0.3g of fluorosilane as a hydrophobic substance, then mechanically stirring at 1000rpm for 1h, then ultrasonically dispersing for 1h under the power of 500Hz, and finally stirring at 60 ℃ for 30min;
(3) and (3) putting the wood into the liquid obtained in the second step, pressurizing for 30min under the pressure of 0.8MPa, recovering to normal pressure, and taking out the wood to finish the super-hydrophobization treatment of the softened wood composite inorganic nano material.
3. Wood compression and densification treatment:
completely covering the upper and lower surfaces (radial sections) of the wood treated in the second step by using two 120-mesh sand papers to enable the rough surface of the sand paper to be in contact with the wood, then placing the wood with the sand paper in a hot press, and compressing the wood to 25% of the original thickness under the conditions of room temperature and 10 MPa; then, gradually heating: firstly heating to 80 ℃ and keeping the pressure for 8h, then continuously heating to 120 ℃ and keeping the pressure for 48h, then cooling the hot press to room temperature at the speed of 20 ℃/h while keeping the pressure, then recovering to normal pressure and removing abrasive paper, and finishing the wood compression and densification treatment, wherein the thickness of the wood is kept to be 25% of the original thickness.
4. High-temperature carbonization treatment of wood:
putting the wood treated in the third step into a high-temperature carbonization box, heating to 150 ℃ at the speed of 5 ℃/h, preserving heat for 3h, then continuously heating to 200 ℃ at the speed of 5 ℃/h, and preserving heat for 48h; then, gradually cooling to 150 ℃ at the speed of 3 ℃/h, preserving heat for 3h, and spraying steam on the wood every 1h for 10min in the heat preservation stage; then, gradually cooling to 120 ℃ at the speed of 5 ℃/h, preserving heat for 3h, and spraying steam on the wood every 1h for 10min in the heat preservation stage; then gradually cooling to 100 ℃ at the speed of 5 ℃/h and preserving heat for 3h; and finally, cooling to room temperature at the speed of 20 ℃/h to obtain the multifunctional carbonized wood.
The microscopic SEM topography of the wood modified by the method shows that the cross section is compressed and compacted, the surface is uniformly distributed with nano silicon dioxide (as shown in figure 1), the diameter section (longitudinal section) is also uniformly distributed with nano silicon dioxide particles, the diameter is about 100nm (as shown in figure 2), the fiber cell wall is in microscopic projection, the whole surface presents a micro-nano structure which is similar to the lotus leaf microstructure, the surface hydrophobic angle of the wood reaches 158 degrees (as shown in figure 3), namely the modified wood has a super-hydrophobic function; the static water contact angle of the radial section of the wood after being rubbed for 20 times by a weight of 100g of sand paper loaded by 240 meshes is as high as 156 degrees and the rolling angle is 8 degrees, and the water absorption capacity of the wood after being continuously soaked in water for 10 days is only 3.2 percent; and the tensile strength, the compressive strength, the impact toughness, the hardness, the wear resistance, the elastic modulus and the static bending strength (table 1) of the modified wood are respectively improved by 6.1 times, 2.58 times, 2.91 times, 3.54 times, 3.1 times, 2.48 times and 2.59 times compared with the untreated wood, the corrosion resistance is improved by 91.4 percent, the heat release rate peak value tested by a cone calorimeter is improved by 11 percent compared with the untreated wood, the oxygen index is improved by 6.1 compared with the untreated wood, and the flame retardant property is obviously improved.
The wood obtained by the treatment method is expected to be used in the fields of building structural materials, sports equipment materials and transportation materials with higher requirements on material strength indoors and outdoors.
Example 2: the preparation method of the multifunctional carbonized wood comprises the following steps:
1. wood softening pretreatment:
putting basswood into a NaOH aqueous solution with the mass concentration of 2wt%, heating for 2h at the temperature of 90 ℃ to remove most hemicellulose, and then washing the basswood to be neutral by distilled water at room temperature to obtain softened wood.
2. Super-hydrophobization treatment of the softened wood composite inorganic nano material:
(1) adding 1g of inorganic nano ferroferric oxide with the mass and the diameter of 30nm into 100ml of toluene, adding 0.6g of polydimethylsiloxane, then ultrasonically dispersing for 1h under the power of 500Hz, and mechanically stirring for 72h at the speed of 1000rpm at room temperature; the mixture was then centrifuged at 6000rpm for 15min and washed repeatedly 3 times successively with dichloromethane and acetone, and after centrifugation at 6000rpm for 15min, it was dried at 100 ℃ for 24h.
(2) Adding the inorganic nano material obtained in the step one into 30g of absolute ethyl alcohol, then dropwise adding 0.3g of fluorosilane serving as a hydrophobic substance into the inorganic nano material, then mechanically stirring the mixture at the speed of 1000rpm for 1 hour, then performing ultrasonic dispersion on the mixture for 1 hour under the power of 500Hz, and finally stirring the mixture for 30min at the temperature of 60 ℃;
(3) and (3) putting the wood into the liquid obtained in the second step, pressurizing for 30min under the pressure of 0.8MPa, recovering to normal pressure, and taking out the wood to finish the super-hydrophobization treatment of the softened wood composite inorganic nano material.
3. Wood compression and densification treatment:
completely covering the upper and lower surfaces (radial sections) of the wood treated in the second step by using two 120-mesh sand papers to enable the rough surface of the sand paper to be in contact with the wood, then placing the wood with the sand paper in a hot press, and compressing the wood to 24% of the original thickness under the conditions of room temperature and 8 MPa; then, gradually heating: firstly heating to 60 ℃ and keeping the pressure for 10h, then continuously heating to 100 ℃ and keeping the pressure for 40h, then cooling the hot press to room temperature at the speed of 15 ℃/h while keeping the pressure, then recovering to normal pressure and removing abrasive paper, and finishing the compression and densification treatment of the wood, wherein the thickness of the wood is kept to be 24% of the original thickness.
4. High-temperature carbonization treatment of wood:
and (3) placing the wood treated in the third step into a high-temperature carbonization box, heating to 140 ℃ at the speed of 8 ℃/h, preserving heat for 3h, then continuously heating to 200 ℃ at the speed of 8 ℃/h, and preserving heat for 40h. Then, gradually cooling to 150 ℃ at the speed of 5 ℃/h, preserving heat for 2h, and spraying steam on the wood every 1h in the heat preservation stage for 10min; then, gradually cooling to 120 ℃ at the speed of 3 ℃/h, preserving heat for 2h, and spraying steam on the wood every 1h in the heat preservation stage for 10min; then the temperature is gradually reduced to 100 ℃ at the speed of 8 ℃/h and is kept for 3h; and finally, cooling to room temperature at the speed of 15 ℃/h to obtain the multifunctional carbonized wood.
The microscopic SEM topography of the wood modified by the method of the invention shows that the cross section is compressed and compacted, nano ferroferric oxide (as shown in figure 4) is uniformly distributed on the surface, nano ferroferric oxide particles are uniformly distributed on the radial section (longitudinal section), the diameter is about 50nm (as shown in figure 5), the fiber cell wall is in a microscopic bulge, the whole surface is in a micro-nano structure similar to the lotus leaf microstructure, the hydrophobic angle of the wood surface reaches 153 degrees (as shown in figure 6), namely the modified wood has the super-hydrophobic function; after the radial section of the wood is rubbed for 20 times by a weight with 100g of sand paper loaded by 240 meshes, the static water contact angle is still as high as 150 degrees and the rolling angle is still 10 degrees, and the water absorption capacity of the wood after being continuously soaked in water for 10 days is only 4.6 percent; the tensile strength, the compressive strength, the impact toughness, the hardness, the wear resistance, the elastic modulus and the static bending strength (table 1) of the modified wood are respectively improved by 6.22 times, 2.63 times, 2.83 times, 3.41 times, 2.91 times, 2.52 times and 2.64 times compared with the untreated wood, the corrosion resistance is improved by 90.6 percent, the heat release rate peak value tested by a cone calorimeter is improved by 12 percent compared with the untreated wood, the oxygen index is improved by 6.6 percent compared with the untreated wood, and the flame retardant property is obviously improved; the magnetic strength can reach 52emu/g, and the magnetic material has high paramagnetism.
The wood obtained by the treatment method is expected to be used in the fields of building structural materials, sports equipment materials and transportation materials with higher requirements on material strength indoors and outdoors.
Example 3: the preparation method of the multifunctional carbonized wood comprises the following steps:
1. wood softening pretreatment:
and (3) carrying out steam jet steaming on the surface of the basswood for 2 hours at the temperature of 120 ℃ to obtain the softened wood.
2. Super-hydrophobization treatment of the softened wood composite inorganic nano material:
(1) adding 1g of inorganic nano silver with the diameter of 20nm into 100ml of toluene, adding 0.6g of polydimethylsiloxane, then performing ultrasonic dispersion for 1h under the power of 500Hz, and mechanically stirring for 72h at the room temperature at the speed of 1000 rpm; the mixture was then centrifuged at 6000rpm for 15min and washed repeatedly 3 times successively with dichloromethane and acetone, and after centrifugation at 6000rpm for 15min, it was dried at 100 ℃ for 24h.
(2) Adding the inorganic nano material obtained in the step one into 30g of absolute ethyl alcohol, then dropwise adding 0.3g of fluorosilane as a hydrophobic substance, then mechanically stirring at 1000rpm for 1h, then ultrasonically dispersing for 1h under the power of 500Hz, and finally stirring at 60 ℃ for 30min;
(3) and (3) putting the wood into the liquid obtained in the second step, pressurizing for 30min under the pressure of 0.8MPa, recovering to normal pressure, and taking out the wood to finish the super-hydrophobization treatment of the softened wood composite inorganic nano material.
3. Wood compression and densification treatment:
completely covering the upper and lower surfaces (radial sections) of the wood treated in the second step by using two 120-mesh sand papers to enable the rough surface of the sand paper to be in contact with the wood, then placing the wood with the sand paper in a hot press, and compressing the wood to 23% of the original thickness under the conditions of room temperature and 10 MPa; then, gradually heating: firstly heating to 70 ℃ and keeping the pressure for 9h, then continuously heating to 120 ℃ and keeping the pressure for 44h, then cooling the hot press to room temperature at the speed of 17 ℃/h under the condition of keeping the pressure, then recovering to normal pressure and removing the sand paper to finish the wood compression and densification treatment, wherein the thickness of the wood is compressed to 23 percent of the original thickness.
4. High-temperature carbonization treatment of wood:
putting the wood treated in the third step into a high-temperature carbonization box, heating to 145 ℃ at the speed of 9 ℃/h, preserving heat for 2.5h, then continuously heating to 195 ℃ at the speed of 9 ℃/h, and preserving heat for 35h; then, gradually cooling to 150 ℃ at the speed of 4 ℃/h, preserving heat for 2.5h, and spraying steam on the wood every 1h for 10min in the heat preservation stage; then, gradually cooling to 120 ℃ at the speed of 4 ℃/h, preserving heat for 3h, and spraying steam on the wood every 1h for 10min in the heat preservation stage; then the temperature is gradually reduced to 100 ℃ at the speed of 9 ℃/h and is kept for 3h; and finally, cooling to room temperature at the speed of 18 ℃/h to obtain the multifunctional carbonized wood.
The microscopic SEM topography of the wood modified by the method of the invention shows that the cross section is compressed and compacted, nano silver is distributed on the surface (as shown in figure 7), nano silver particles are uniformly distributed on the radial section (longitudinal section), the diameter is about 20nm (as shown in figure 8), the hydrophobic angle of the wood surface reaches 154 degrees (as shown in figure 9), namely, the modified wood has the super-hydrophobic function; after the radial section of the wood is rubbed for 20 times by a weight with 100g of sand paper loaded by 240 meshes, the static water contact angle is still as high as 151 degrees and the rolling angle is 9 degrees, and the water absorption capacity of the wood after being continuously soaked in water for 10 days is only 4.3 percent; and the tensile strength, the compressive strength, the impact toughness, the hardness, the wear resistance, the elastic modulus and the static bending strength (table 1) of the modified wood are respectively improved by 5.61 times, 2.54 times, 2.68 times, 3.25 times, 2.88 times, 2.41 times and 2.52 times compared with the untreated wood, the corrosion resistance is improved by 94.8 percent, the heat release rate peak value tested by a cone calorimeter is improved by 10 percent compared with the untreated wood, the oxygen index is improved by 5.7 compared with the untreated wood, and the flame retardant property is obviously improved.
The wood obtained by the treatment method is expected to be used in the fields of building structural materials, sports equipment materials and transportation materials with higher requirements on material strength indoors and outdoors.
Example 4: the preparation method of the functional carbonized wood of the embodiment comprises the following steps:
1. wood softening pretreatment:
putting basswood into a NaOH aqueous solution with the mass concentration of 2wt%, heating for 2h at the temperature of 90 ℃ to remove most hemicellulose, and then washing the basswood to be neutral by distilled water at room temperature to obtain softened wood.
2. Super-hydrophobization treatment of the softened wood composite inorganic nano material:
(1) adding a two-dimensional inorganic boron nitride lamellar raw material with the mass of 1g, the side length of 30 mu m and the thickness of 5 mu m into 100ml of toluene, adding 0.6g of polydimethylsiloxane, and then ultrasonically dispersing for 1h under the power of 500Hz, wherein the boron nitride is dispersed into a two-dimensional lamellar material with the length of several micrometers and the thickness of several to dozens of nanometers; then mechanically stirring for 72 hours at room temperature at the speed of 1000 rpm; then, the mixture was centrifuged at 6000rpm for 15min, and repeatedly washed with dichloromethane and acetone 3 times in succession, and after centrifugation at 6000rpm for 15min, the mixture was dried at 100 ℃ for 24 hours.
(2) Adding the inorganic nano material obtained in the step one into 30g of absolute ethyl alcohol, then dropwise adding 0.3g of fluorosilane as a hydrophobic substance, then mechanically stirring at 1000rpm for 1h, then ultrasonically dispersing for 1h under the power of 500Hz, and finally stirring at 60 ℃ for 30min;
(3) and (3) putting the wood into the liquid obtained in the second step, pressurizing for 30min under the pressure of 0.8MPa, recovering to normal pressure, and taking out the wood to finish the super-hydrophobization treatment of the softened wood composite inorganic nano material.
3. Wood compression and densification treatment:
completely covering the upper and lower surfaces (radial sections) of the wood treated in the second step by using two 120-mesh abrasive paper to enable the rough surface of the abrasive paper to be in contact with the wood, then placing the wood with the abrasive paper in a hot press, and compressing the wood to 24% of the original thickness under the conditions of room temperature and 8 MPa; and then gradually heating: firstly heating to 60 ℃ and keeping the pressure for 10h, then continuously heating to 100 ℃ and keeping the pressure for 40h, then cooling the hot press to room temperature at the speed of 15 ℃/h while keeping the pressure, then recovering to normal pressure and removing abrasive paper, and finishing the compression and densification treatment of the wood, wherein the thickness of the wood is kept to be 24% of the original thickness.
4. High-temperature carbonization treatment of wood:
putting the wood treated in the third step into a hot press, heating to 200 ℃ at the speed of 10 ℃/h under the pressure of 8MPa in the third step, and preserving heat for 24h; then, gradually cooling to 150 ℃ at the speed of 5 ℃/h, preserving heat for 2h, and spraying steam on the wood every 1h in the heat preservation stage for 10min; then, gradually cooling to 120 ℃ at the speed of 3 ℃/h, preserving heat for 2h, and spraying steam on the wood every 1h in the heat preservation stage for 10min; then the temperature is gradually reduced to 100 ℃ at the speed of 8 ℃/h and is kept for 3h; and finally, cooling to room temperature at the speed of 15 ℃/h to obtain the multifunctional carbonized wood.
The microscopic SEM-EDX topography of the wood modified by the method of the invention shows that the cell cavities of the radial section present dispersed two-dimensional layered nano boron nitride (as a dotted line area in figure 10), the length dimension is about 2-3 microns, which shows that the boron nitride has been dispersed by ultrasonic, the cells on the transverse section are compressed and compacted (as figure 11), the hydrophobic angle of the radial section of the wood reaches 152 degrees (as figure 12), namely the modified wood has the super-hydrophobic function, and the energy spectrum scanning surface boron nitride corresponding to the transverse section is compressed and limited in the wood (as figure 13, the A is N element, and the B is B element); the static water contact angle of the radial cut surface of the wood after being rubbed for 20 times by a weight of 100g of sand paper loaded with 240 meshes is still as high as 150 degrees and the rolling angle is still 10 degrees, and the water absorption capacity of the wood after being continuously soaked in water for 10 days is only 3.6 percent; and the tensile strength, the compressive strength, the impact toughness, the hardness, the wear resistance, the elastic modulus and the static bending strength (table 1) of the modified wood are respectively improved by 5.94 times, 3.12 times, 2.92 times, 4.32 times, 3.37 times, 3.15 times and 2.96 times compared with the untreated wood, the corrosion resistance is improved by 90.7 percent, the heat release rate peak value tested by a cone calorimeter is improved by 15 percent compared with the untreated wood, the oxygen index is improved by 8.2 compared with the untreated wood, and the flame retardant property is obviously improved.
The wood obtained by the treatment method is expected to be used in the fields of building structural materials, sports equipment materials and transportation materials with higher requirements on material strength indoors and outdoors.
Table 1 comparison of mechanical properties of untreated basswood wood and modified wood of different embodiments
Remarking: the mechanical properties were tested according to GB/T1928-2009, each value being the mean of three measurements.
Claims (5)
1. The preparation method of the multifunctional carbonized wood is characterized by comprising the following steps:
1. wood softening pretreatment:
softening and pretreating the wood by adopting a steaming method, an alkali treatment method or a steaming method;
2. super-hydrophobization treatment of the softened wood composite inorganic nano material:
(1) adding inorganic nano material with the diameter or thickness of 1-100nm into toluene, adding polydimethylsiloxane, then ultrasonically dispersing for 1-1.5 h at 500-550 Hz, and mechanically stirring for 70-74 h at the room temperature of 1000-1200 rpm; centrifuging for 15-30 min, repeatedly washing with dichloromethane and acetone for 3-5 times, centrifuging for 15-30 min, and drying for 22-26 h; wherein the volume ratio of the mass of the inorganic nano material to the toluene is 1g: (90-110) mL, wherein the mass ratio of the inorganic nano material to the polydimethylsiloxane is 1 (0.5-0.7);
the inorganic nano material is nano silicon dioxide, nano titanium dioxide, nano silver, nano zinc oxide, nano ferroferric oxide, nano calcium carbonate, two-dimensional nano clay, two-dimensional nano boron nitride, two-dimensional graphene or two-dimensional graphene oxide;
(2) adding the inorganic nano material treated in the step one into absolute ethyl alcohol, then dropwise adding fluorosilane serving as a hydrophobic substance into the absolute ethyl alcohol, then mechanically stirring for 1-1.5 hours, then performing ultrasonic dispersion, and finally stirring and treating for 30-40 min at the temperature of 60-65 ℃ to obtain liquid;
(3) putting wood into the liquid obtained in the step (2), pressurizing for 30-40 min under the pressure of 0.8-0.9 MPa, recovering to normal pressure, and taking out the wood to finish the super-hydrophobization treatment of the softened wood composite inorganic nano material; the mass ratio of the inorganic nano material to the absolute ethyl alcohol is 1 (29-31), and the mass ratio of the inorganic nano material to the fluorosilane is 1 (0.2-0.4);
3. wood compression and densification treatment:
completely covering the upper and lower surfaces of the longitudinal section of the wood treated in the second step by using two 120-mesh sand papers to enable the rough surface of the sand paper to be in contact with the wood, then placing the wood with the sand paper in a hot press, and compressing the wood to 20-25% of the original thickness under the conditions of room temperature and 5-10 MPa; then, gradually heating: firstly heating to 60-80 ℃ and keeping the pressure for 8-10h, then continuously heating to 100-120 ℃ and keeping the pressure for 24-48h, then cooling the hot press to room temperature at the speed of 20 ℃/h while keeping the pressure, then recovering to normal pressure and removing abrasive paper to finish the compression and densification treatment of the wood;
4. wood high-temperature carbonization:
putting the wood treated in the third step into a high-temperature carbonization box, heating to 130-150 ℃ at the speed of 5-10 ℃/h, preserving heat for 2-3h, then continuously heating to 180-200 ℃ at the speed of 5-10 ℃/h, and preserving heat for 24-48h; or continuously placing the mixture in a hot press, heating to 180-200 ℃ at the speed of 5-10 ℃/h under the pressure of 5-10MPa in the third step, and preserving heat for 24-48h;
then, gradually cooling to 150 ℃ at the speed of 3-5 ℃/h, preserving heat for 2-3h, and spraying steam on the wood every 1h in the heat preservation stage for 10min; then, gradually cooling to 120 ℃ at the speed of 3-5 ℃/h, preserving heat for 2-3h, and spraying water vapor on the wood every 1h in the heat preservation stage for 10min; then the temperature is gradually reduced to 100 ℃ at the speed of 5-10 ℃/h and is kept for 2-3h; and finally, cooling to room temperature at the speed of 10-20 ℃/h to obtain the multifunctional carbonized wood.
2. The method for preparing a multifunctional carbonized wood as described in claim 1, wherein the steaming process comprises soaking wood in distilled water, heating to 100 deg.C, and steaming for 2 hr to obtain softened wood.
3. The method for preparing multifunctional carbonized wood according to claim 1, wherein the alkali treatment process comprises placing wood in 2% by mass concentration NaOH aqueous solution, heating at 90 ℃ for 2h to remove most of hemicellulose, and washing with distilled water at room temperature to neutrality to obtain softened wood.
4. The method for preparing the multifunctional carbonized wood according to claim 1, wherein the steaming method is to steam the surface of the wood with water vapor at a temperature of 120 ℃ for 2 hours to obtain softened wood.
5. The method for preparing a multifunctional carbonized wood according to claim 1, characterized in that the fluorosilane in the step two (3) is one or a mixture of several of heptadecafluorosilyltrimethoxysilane, heptadecafluorosilyltriethoxysilane, tridecafluorosilyltrimethoxysilane and tridecafluorosilyltriethoxysilane in any ratio.
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