CN108527572B - Transparent wood with optical regulation and control function and preparation method thereof - Google Patents
Transparent wood with optical regulation and control function and preparation method thereof Download PDFInfo
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- CN108527572B CN108527572B CN201710128873.4A CN201710128873A CN108527572B CN 108527572 B CN108527572 B CN 108527572B CN 201710128873 A CN201710128873 A CN 201710128873A CN 108527572 B CN108527572 B CN 108527572B
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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
- 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
- B27K3/0207—Pretreatment of wood before 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
- 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
- B27K3/0207—Pretreatment of wood before impregnation
- B27K3/0214—Drying
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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
- B27K3/15—Impregnating involving polymerisation including use of polymer-containing impregnating agents
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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
- B27K3/52—Impregnating agents containing mixtures of inorganic and organic compounds
-
- 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
- B27K5/003—Treating of wood not provided for in groups B27K1/00, B27K3/00 by using electromagnetic radiation or mechanical waves
- B27K5/0055—Radio-waves, e.g. microwaves
Abstract
The invention relates to a transparent wood with an optical regulation function and a preparation method thereof, wherein the transparent wood comprises a transparent wood matrix and inorganic particles with the optical regulation function uniformly dispersed in the transparent wood matrix, and the inorganic particles with the optical regulation function are selected from at least one of nano silver, nano vanadium oxide, nano cesium tungstate, nano ATO and nano ITO. The invention utilizes the characteristic of high haze of the transparent wood, increases the transmission channel of light in the transparent wood matrix and improves the functional benefit of the inorganic nano-particles with the same concentration.
Description
Technical Field
The invention relates to a preparation process of a composite material, and particularly belongs to the technical field of organic-inorganic compounding.
Background
The variety of plants is many, and the variety of wood is also eight-flower. For the past several thousand years, wood has been used by people as building materials or fuel. However, the research on wood composite materials has just started. The wood composite material not only can make high-efficiency use of low-quality wood, small-diameter wood, waste wood and agricultural residues, but also has a fresh and well-known ecological effect (1) Lishunlong, forest carbon sink problem research, Harbin, northeast forestry university Press, 2006).
In 2007, Yano professor of Tokyo university utilizes wood fiber and high molecular polymer to compound, and transparent high-strength paper is manufactured in a laboratory environment, the technology is very similar to a papermaking process, the visible light transmittance of the transparent paper is basically equal to that of a commercial PET film, the elastic modulus is 4-5 times of that of the commercial PET film, and the breaking tensile strength can reach 2-3 times of that of the commercial PET film (2 H.Yano. (nanometer level) nanoscale.3(2011) 71-85). Professor Lars of royal university of physical engineering in sweden originally proposed the concept of transparent wood, moved the field of wood research, opened a skylight of new material, his inspiration came from the traditional papermaking process in our country, and filled polymethyl methacrylate in the pores of lignin-free lignocellulose, professor Lars made transparent wood in the laboratory with visible light transmittance up to 80% ([3] b.lars. (biomacromolecule) biomacromolecules.17(2016) 1358-1364). In the same year, the chinese scientist hui professor at the university of maryland, usa, filled the pores of delignified wood with epoxy resin, which, due to its refractive index of visible light closer to that of lignocellulose fiber, gave a composite material filled with epoxy resin with a visible light transmittance of up to 90% ([4] l.hu. (advanced material) adv.mater.28(2016) 5181-5187). However, the transparent wood materials reported at present only have the advantages of high strength, high transparency and high haze, and the functionalized products of the transparent wood materials are yet to be further researched and developed.
Disclosure of Invention
The invention aims to provide transparent wood with an optical regulation and control function and a preparation method thereof.
In one aspect, the invention provides transparent wood with an optical regulation and control function, which comprises a transparent wood matrix and inorganic particles with an optical regulation and control function uniformly dispersed in the transparent wood matrix, wherein the inorganic particles with an optical regulation and control function are selected from at least one of nano silver, nano vanadium oxide, nano cesium tungstate, nano ATO and nano ITO.
The invention combines the inorganic particles with the optical regulation function with the transparent wood matrix for the first time to obtain the transparent wood with the optical regulation function. The invention utilizes the characteristic of high haze of the transparent wood, increases the transmission channel of light in the transparent wood matrix and improves the functional benefit of the inorganic nano-particles with the same concentration.
Preferably, the content of the inorganic particles with optical control function in the transparent wood with optical control function is 0.01-0.04 wt%. The addition of the inorganic particles in the range can not influence the mechanical strength of the transparent wood matrix, and the high-concentration inorganic particles can have agglomeration phenomenon, so that stress concentration is formed when the inorganic particles are subjected to external force, and the mechanical strength of the transparent wood is reduced; and the optical regulation and control function effect of the inorganic particles with low concentration is not obvious.
Preferably, the grain size of the inorganic particles with the optical regulation function is 10-50 nm, and the visible light transmission performance of the transparent wood matrix is not affected by the inorganic particles within the range.
Preferably, the transparent wood matrix comprises a delignified wood matrix and a high molecular polymer distributed in a pore structure of the delignified wood matrix, wherein the high molecular polymer is polymethyl methacrylate, epoxy resin or polydimethylsiloxane.
In another aspect, the invention further provides a preparation method of the transparent wood with the optical control function, which comprises the following steps:
dispersing inorganic particles with an optical regulation function in a high molecular polymer monomer solution to obtain a dispersion liquid A;
and injecting the obtained dispersion liquid A into the delignified wood matrix, and then initiating a polymerization reaction of a high-molecular polymer monomer in the delignified wood matrix to obtain the transparent wood with the optical regulation function.
The invention adopts the method of dispersing inorganic particles with the optical regulation function in the high molecular polymer monomer solution and then injecting the inorganic particles into the delignified wood to obtain the transparent wood with the optical regulation function, and has simple production process and low requirement on equipment. The main raw material used in the method is wood, and the method is low in cost and renewable. The prepared composite material has very high strength, better transparency and specific optical regulation performance.
Preferably, the lignin in the wood matrix is removed through chemical treatment, and then the lignin-removed wood matrix is obtained through hydrophobic oleophylic modification treatment and drying treatment.
Preferably, the chemical treatment is to place the wood substrate in a chemical reagent to react for 1-10 hours at 25-100 ℃, wherein the chemical reagent is at least one selected from hydrogen peroxide, a mixed solution of sodium hypochlorite and sodium hydroxide and perchloric acid.
Preferably, the hydrophobic and oleophylic modification treatment is to immerse the chemically treated delignified wood matrix into a solution containing a modifier, wherein the concentration of the modifier in the solution containing the modifier is 0.01-0.1 mol/L, and the modifier is n-octadecanethiol, n-dodecanethiol or stearic acid, and the reaction is carried out for 12-24 hours.
Further, the drying treatment is preferably freeze drying, vacuum drying or supercritical drying.
Preferably, the method of injection is a full cell method or a semi-limiting method. The full cell method comprises the following steps: placing the hydrophobic and oleophilic delignified wood matrix in a container for vacuum treatment, adding a high molecular polymer monomer solution until the container is filled with the hydrophobic and oleophilic delignified wood matrix, and removing the vacuum; and then pressurizing to 1-3MPa until the immersion amount of the high molecular polymer monomer solution is saturated, and recovering to normal pressure after vacuum treatment. The vacuum degree of the vacuum treatment is preferably 79 to 86kPa, and the time is preferably 15 minutes to 2 hours, more preferably 1 to 2 hours. Specifically, the hydrophobic and oleophilic delignified wood matrix is placed in a treatment tank and then subjected to vacuum treatment, wherein the vacuum degree is generally 79-86 kPa, and the treatment tank is kept for 15-60 min. After the vacuum reaches a certain degree, adding the high molecular polymer monomer solution, and keeping the vacuum degree unchanged so as to avoid uneven injection of the high molecular polymer monomer solution; and (3) after the treatment tank is filled with the high molecular polymer monomer solution, releasing the vacuum, starting pressurizing to the maximum pressure (1-3 MPa), and then keeping the maximum pressure until the immersion amount is saturated. After pressure is relieved, high molecular polymer monomer solution can be by the inside gas "recoil" that persists of a small amount of wood, with high molecular polymer monomer solution discharge back, the processing jar still need the evacuation again, fills the hole that exists in the wood through the high molecular polymer monomer solution who retrieves wood surface. Maintaining the vacuum for a period of time, and releasing the vacuum. The semi-limiting method comprises the following steps: and (3) placing the hydrophobic and oleophilic delignified wood matrix into a container filled with a high molecular polymer monomer solution, pressurizing to 1-3MPa until the immersion amount of the high molecular polymer monomer solution is saturated, and recovering to normal pressure after vacuum treatment. The vacuum degree of the vacuum treatment is preferably 79 to 86kPa, and the time is preferably 15 minutes to 2 hours, more preferably 1 to 2 hours. Specifically, after the hydrophobic and oleophilic delignified wood matrix is placed in a treatment tank, the treatment tank is filled with a high molecular polymer monomer solution, the treatment tank starts to pressurize to the maximum pressure (1-3 MPa), and then the maximum pressure is maintained until the immersion amount is saturated. After pressure is relieved, high molecular polymer monomer solution can be by the inside gas "recoil" that persists of a small amount of wood, with high molecular polymer monomer solution discharge back, the processing jar still need the evacuation again, fills the hole that exists in the wood through the high molecular polymer monomer solution who retrieves wood surface. Maintaining the vacuum for a period of time, and releasing the vacuum.
Preferably, the high molecular polymer monomer solution is a methyl methacrylate solution, a bisphenol A glycidyl ether solution or a dimethyl siloxane solution.
Preferably, the high molecular polymer monomer is initiated to carry out polymerization reaction by ultraviolet irradiation or heating at 50-80 ℃, wherein the power of the ultraviolet irradiation is 10-30W, and the time is 1-3 hours.
Preferably, the concentration of the inorganic particles in the dispersion liquid A is 0.03-0.1 wt%.
The method has the advantages of low cost of required raw materials, simple process and easy batch production. The functional transparent wood material prepared by the method has high strength, good transparency and optical regulation and control performance.
Drawings
FIG. 1 is a digital photograph of transparent wood having a near infrared shielding function in example 1;
FIG. 2 is an optical transmittance curve of transparent wood having a near infrared shielding function in example 1;
FIG. 3 is a digital photograph of the transparent wood with intelligent temperature adjusting function in example 2;
fig. 4 is an optical transmittance curve of the transparent wood with intelligent temperature adjusting function in example 2;
FIG. 5 is a digital photograph of transparent wood having middle and far infrared shielding function in example 3;
FIG. 6 is an optical transmittance curve of transparent wood having middle and far infrared shielding function in example 3;
FIG. 7 is a stress-strain curve of the transparent wood having optical control function in examples 1 to 3;
fig. 8 is an optical transmittance curve of the transparent wood having a near infrared shielding function in comparative example 1.
Detailed Description
The present invention is further illustrated by the following examples, which are to be understood as merely illustrative and not restrictive.
In the invention, the transparent wood with the optical regulation and control function comprises a transparent wood matrix and inorganic particles with the optical regulation and control function uniformly dispersed in the transparent wood matrix, wherein the inorganic particles with the optical regulation and control function are selected from at least one of nano silver, nano vanadium oxide, nano cesium tungstate, nano ATO (antimony doped tin oxide) and nano ITO (indium doped tin oxide). The content of the inorganic particles with the optical regulation function in the transparent wood with the optical regulation function can be 0.01-0.1 wt%, the addition of the inorganic particles in the range does not influence the mechanical strength of the transparent wood matrix, and the mass content of the high molecular polymer can be 30-70 wt%. The grain size of the inorganic particles with the optical regulation function can be 10-50 nm. Wherein, transparent wood base member is including delignification wood base member and distribute in the macromolecular polymer in the pore structure of delignification wood base member, macromolecular polymer is polymethyl methacrylate, epoxy or polydimethylsiloxane.
The invention firstly disperses inorganic particles with optical regulation function in high molecular polymer monomer solution. The resulting dispersion was then injected into delignified wood. Finally, high molecular polymer is initiated to polymerize, and the transparent wood with the optical regulation function is obtained. The following exemplarily illustrates a method for preparing the transparent wood having an optical control function according to the present invention.
Preparing the delignified wood matrix. The lignin in the wood matrix is removed through chemical treatment, and the lignin-removed wood matrix is obtained after drying treatment. Or removing lignin in the wood matrix through chemical treatment, and then performing hydrophobic oleophylic modification treatment and drying treatment to obtain the lignin-removed wood matrix. The method for preparing the delignified wood matrix according to the present invention includes not only the above two methods.
Removing lignin in the wood matrix through chemical treatment to obtain the lignin-removed wood matrix. Specifically, the lignin in wood is removed by a chemical reagent soaking method, namely, the wood matrix is placed in the chemical reagent to react for 1-10 hours at 25-100 ℃. The chemical agent can be at least one selected from hydrogen peroxide, sodium hypochlorite and sodium hydroxide mixed solution or perchloric acid. Wherein the concentration of the hydrogen peroxide can be 15 wt% -30 wt%. The concentration of perchloric acid can be from 12 to 15% by weight. In the mixed solution of sodium hypochlorite and sodium hydroxide, the concentration of the sodium hypochlorite can be 3 wt% -5 wt%, and the concentration of the sodium hydroxide can be 15 wt% -20 wt%.
And immersing the delignified wood matrix subjected to chemical treatment into a solution containing a modifier for reaction for 12-24 hours, wherein the concentration of the modifier in the solution containing the modifier is 0.01-0.1 mol/L. The organic solvent in the solution containing the modifier can be ethanol, isopropanol, toluene, ethyl acetate and the like. Or washing the chemically treated delignified wood matrix with the organic solvent (e.g., ethanol, isopropanol, toluene, ethyl acetate, etc.) prior to immersion in the solution containing the modifier to remove the chemical agents present in the delignified wood matrix. As an example, the chemically treated lignin-removed wood head matrix is cleaned by ethanol and soaked in an ethanol solution of a modifier for reaction for 12-24 hours, wherein the modifier is n-octadecanethiol, n-dodecanethiol or stearic acid. Then drying treatment is carried out to remove lignin from the wood matrix.
And drying the chemically treated wood substrate. The drying treatment may be freeze drying, vacuum drying or supercritical drying. In particular, the chemically treated wood matrix is freeze-dried, vacuum-dried or super-critical dried without destroying the pore structure of the wood. Wherein, the vacuum drying can use a vacuum drying oven, the vacuum degree is 100Pa to 200Pa, and the temperature is 80 ℃ to 100 ℃. Supercritical drying may be performed using a supercritical carbon dioxide extraction apparatus. The freeze drying may be at-20 deg.C to-40 deg.C for 6-12 hr.
Dispersing inorganic particles with an optical regulation function in one solution of methyl methacrylate, bisphenol A glycidyl ether and dimethyl siloxane to obtain a dispersion liquid A. The concentration of inorganic nanoparticles (inorganic particles) in the dispersion A can be 0.01 wt% to 0.1 wt%. The inorganic particles with the optical regulation function can be at least one of nano silver, nano vanadium oxide, nano cesium tungstate, nano ATO or nano ITO, and the grain size is 10-50 nm.
The dispersion A is injected into the delignified wood matrix by a special method. Specifically, dispersion A was injected into a delignified wood matrix by the full cell method or the half-limiting method to obtain product B. The full cell method is to enter the lignin-removed wood subjected to hydrophobic oleophylic and drying treatment into a treatment tank for vacuumizing, wherein the vacuum degree is 79-86 kPa, and the wood is kept for 15-60 min. And then, after the treatment tank is filled with the methyl methacrylate solution, releasing the vacuum, starting pressurizing to 1-3MPa, and keeping for 15-60 min. And after the pressure is relieved, vacuumizing the treatment tank again, keeping the vacuum for 1-2 hours, and finally relieving the vacuum, wherein the vacuum degree is 79-86 kPa. Wherein the semi-limiting injection method comprises the steps of immersing the lignin-removed wood subjected to hydrophobic oleophylic and drying treatment into methyl methacrylate solution for 1-2h, pressurizing to 1-3Mpa, keeping for 15-60min, vacuumizing to 79-86 kPa, keeping for 1-2h, and returning to normal pressure.
And (4) initiating the polymerization of the high molecular polymer monomer in the product B to obtain the transparent wood with the optical regulation function, and obtaining a finished product. And finally, heating to initiate the polymerization of the high molecular polymer under ultraviolet irradiation (the irradiation power is 10-30W and the irradiation time is 1-3 h) or at the temperature of 50-80 ℃, wherein the polymerization time is 6-24 h, and obtaining the transparent wood with the optical regulation function.
As an example, (1) 100ml of a mixed solution of sodium hypochlorite and sodium hydroxide having a concentration of 5 wt% and 20 wt% was prepared. (2) And (2) cleaning the wood obtained in the step (1) by using ethanol, soaking the wood in an ethanol solution of n-octadecanethiol for reaction for 12 hours, and then drying the wood in a vacuum dryer, wherein the vacuum degree of the vacuum dryer is 100-200 Pa, the drying temperature is 80-100 ℃, and the drying time is 20-24 hours. (3) And (3) immersing the wood obtained in the step (2) into an epoxy resin solution dispersed with cesium tungstate nano particles for 2h, pressurizing to 3MPa, keeping for 15min, vacuumizing to 80kPa, keeping for 2h and recovering to normal pressure. (4) And heating and curing the obtained compound at 60 ℃ for 12h to finally obtain the transparent wood material with the near-infrared shielding function.
The present invention will be described in detail by way of examples. It is also to be understood that the following examples are illustrative of the present invention and are not to be construed as limiting the scope of the invention, and that certain insubstantial modifications and adaptations of the invention by those skilled in the art may be made in light of the above teachings. The specific process parameters and the like of the following examples are also only one example of suitable ranges, i.e., those skilled in the art can select the appropriate ranges through the description herein, and are not limited to the specific values exemplified below.
Example 1
Beech 3cm long, 3cm wide and 0.5cm thick was soaked in 30 wt% hydrogen peroxide solution at 80 deg.C for 4 h. The obtained delignified wood is washed by ethanol, soaked in ethanol solution of n-octadecanethiol (the concentration of the n-octadecanethiol is 0.05mol/L) for reaction for 12 hours, and dried in a vacuum drier (the vacuum degree of a vacuum drying oven is 200Pa, the drying temperature is 80 ℃, and the drying time is 20 hours). Immersing the delignified wood subjected to hydrophobic oleophylic and drying treatment into a methyl methacrylate solution dispersed with 0.03 wt% of cesium tungstate nanoparticles (the particle size is 10-50 nm), pressurizing to 3MPa, keeping for 15min, vacuumizing to 80kPa, keeping for 2h, and returning to normal pressure. And heating and curing the obtained compound at 60 ℃ for 12h to finally obtain the transparent wood material with the near-infrared shielding function, wherein the content of the inorganic particles with the optical control function in the transparent wood material is 0.01 wt%, and the content of the polymethyl methacrylate is 37.5 wt%.
Example 2
Willow of 3cm length, 3cm width and 0.5cm thickness is soaked in a mixed solution of 5 wt% sodium hypochlorite and 20 wt% sodium hydroxide at 100 deg.C for 5 hr. The obtained delignified wood is washed by ethanol, soaked in ethanol solution of n-octadecanethiol (the concentration of the n-octadecanethiol is 0.05mol/L) for reaction for 12 hours, and dried in a vacuum drier (the vacuum degree of a vacuum drying oven is 200Pa, the drying temperature is 80 ℃, and the drying time is 20 hours). Soaking the delignified wood (delignified wood matrix) subjected to hydrophobic oleophylic and drying treatment into an epoxy resin solution (the monomer of the epoxy resin solution is bisphenol A glycidyl ether) dispersed with 0.05 wt% of vanadium oxide nanoparticles (the particle size is 10-50 nm) and pressurizing to 3MPa for 15min, then vacuumizing to 80kPa and maintaining for 2h and recovering to normal pressure. And heating and curing the obtained compound at 60 ℃ for 12h to finally obtain the transparent wood material with the intelligent temperature-regulating function, wherein the content of the inorganic particles with the optical regulating function in the transparent wood material is 0.03 wt%, and the content of the epoxy resin is 60.5 wt%.
Example 3
A basswood 3cm long, 3cm wide and 0.5cm thick is soaked in a perchloric acid solution 15 wt% at 90 deg.C for 5 h. The obtained delignified wood is washed by ethanol, soaked in ethanol solution of n-octadecanethiol (the concentration of the n-octadecanethiol is 0.05mol/L) for reaction for 12 hours, and dried in a vacuum drier (the vacuum degree of a vacuum drying oven is 200Pa, the drying temperature is 80 ℃, and the drying time is 20 hours). Soaking the delignified wood subjected to hydrophobic oleophylic treatment and drying in an epoxy resin solution (the monomer of which is bisphenol A glycidyl ether) dispersed with 0.1wt% of silver nanoparticles (the particle size is 10-50 nm) to be pressurized to 3MPa and kept for 15min, and then vacuumizing to 80kPa and keeping for 2h and restoring to normal pressure. And heating and curing the obtained compound at 60 ℃ for 12h to finally obtain the transparent wood material with the middle and far infrared shielding function, wherein the content of the inorganic particles with the optical control function in the transparent wood material is 0.04wt%, and the content of the epoxy resin is 40.1 wt%.
Fig. 1 to 2 are a digital photograph and an optical transmittance curve of the transparent wood material having a near infrared shielding function according to example 1, respectively. From fig. 1-2, it can be seen that the transmittance of the transparent wood material with the near-infrared shielding function to 550nm visible light is 80%, and the transmittance to 1500nm near-infrared light is only 2%.
Fig. 3 to 4 are a digital photograph and an optical transmittance curve of the transparent wood material with the smart temperature adjusting function in example 2, respectively, and it can be seen from fig. 3 to 4 that the transparent wood material with the smart temperature adjusting function is transparent to near infrared light at Tc temperature (68 ℃) or lower and shielding to near infrared light at Tc temperature (68 ℃) or higher.
Fig. 5 to 6 are a digital photograph and an optical transmittance curve of the transparent wood material having the middle and far infrared shielding function according to example 3, respectively. From fig. 5-6, it can be seen that the transparent wood material with middle and far infrared shielding function has certain shielding performance for middle and far infrared light of 2 μm to 16 μm.
FIG. 7 is a stress-strain curve of the transparent wood material of examples 1-3. From fig. 7, it can be seen that the transparent wood material is a high-strength material, the breaking tensile stress can reach 59.8Mpa, and the elastic modulus can reach 2.72 GPa. Wherein the tensile stress of the transparent wood material in examples 1-3 is 59.8MPa, 59.6MPa, 59.5MPa, respectively, and the elastic modulus is 2.72GPa, 1.96GPa, 1.77GPa, respectively.
Example 4
Beech 3cm long, 3cm wide and 0.5cm thick was soaked in 30 wt% hydrogen peroxide solution at 80 deg.C for 4 h. The obtained delignified wood is washed by ethanol, soaked in ethanol solution of n-octadecanethiol (the concentration of the n-octadecanethiol is 0.05mol/L) for reaction for 12 hours, and dried in a vacuum drier (the vacuum degree of a vacuum drying oven is 200Pa, the drying temperature is 80 ℃, and the drying time is 20 hours). Immersing the delignified wood subjected to hydrophobic oleophylic and drying treatment into a methyl methacrylate solution dispersed with 0.1wt% of cesium tungstate nano particles (the particle size is 10-50 nm), pressurizing to 3MPa, keeping for 15min, vacuumizing to 80kPa, keeping for 2h, and returning to normal pressure. And heating and curing the obtained compound at 60 ℃ for 12h to finally obtain the transparent wood material with the near-infrared shielding function, wherein the content of the inorganic particles with the optical control function in the transparent wood material is 0.03 wt%, and the content of the polymethyl methacrylate is 37.5 wt%. The tensile stress is 52.5Mpa, and the elastic modulus is 2.03 GPa.
Comparative example 1
Beech 3cm long, 3cm wide and 0.5cm thick was soaked in 30 wt% hydrogen peroxide solution at 80 deg.C for 4 h. The obtained delignified wood is washed by ethanol, soaked in ethanol solution of n-octadecanethiol (the concentration of the n-octadecanethiol is 0.05mol/L) for reaction for 12 hours, and dried in a vacuum drier (the vacuum degree of a vacuum drying oven is 200Pa, the drying temperature is 80 ℃, and the drying time is 20 hours). Soaking the delignified wood subjected to hydrophobic oleophylic and drying treatment into methyl methacrylate solution, pressurizing to 3MPa, keeping for 15min, vacuumizing to 80kPa, keeping for 2h and returning to normal pressure. The obtained compound is heated and cured for 12 hours at the temperature of 60 ℃, and finally the transparent wood material is obtained. According to the mass ratio of ethanol: collodion: preparing a coating solution according to the proportion of 1.0:0.93:0.15 of cesium tungstate nano particles, and coating the coating solution on the surface of a transparent wood material by using a coating device, thereby finally obtaining the transparent wood material with the near-infrared shielding function, wherein the contents of polymethyl methacrylate and inorganic particles with the optical control function in the transparent wood material are the same as those in example 1.
Fig. 8 is an optical transmittance curve of transparent wood having a near infrared shielding function. As can be seen from FIG. 8, the transmittance of the transparent wood material with near-infrared shielding function in the comparative example for 550nm visible light is 80%, and the transmittance for 1500nm near-infrared light is higher, namely 36%. The near-infrared shielding function is inferior to that of example 1, which shows that the optical control function of the inorganic nanoparticles can be better improved after the inorganic nanoparticles with the optical control function are dispersed in the polymer monomer solution and injected into the wood matrix by the full cell method or the semi-immersion method.
Comparative example 2
Beech 3cm long, 3cm wide and 0.5cm thick was soaked in 30 wt% hydrogen peroxide solution at 80 deg.C for 4 h. The obtained delignified wood was washed with ethanol and soaked in an ethanol solution of n-octadecanethiol (concentration 0.05mol/L) for 12h and dried in a vacuum drier (vacuum degree of a vacuum drying oven of 200Pa, drying temperature of 80 ℃ C., drying time of 20 h). Soaking the delignified wood subjected to hydrophobic oleophylic and drying treatment into methyl methacrylate solution, pressurizing to 3MPa, keeping for 15min, vacuumizing to 80kPa, keeping for 2h and returning to normal pressure. And heating and curing the obtained compound at 60 ℃ for 12h to finally obtain the transparent wood material with the near-infrared shielding function, wherein the content of the inorganic particles with the optical control function in the transparent wood material is 0 wt%, and the content of the polymethyl methacrylate is 37.6 wt%. The tensile stress is 60.1Mpa, the elastic modulus is 2.73GPa, and the optical regulation function is not provided.
Claims (5)
1. A preparation method of transparent wood with optical regulation and control functions is characterized in that the transparent wood with optical regulation and control functions comprises a transparent wood matrix and inorganic particles with optical regulation and control functions uniformly dispersed in the transparent wood matrix, wherein the inorganic particles with optical regulation and control functions are selected from at least one of nano silver, nano vanadium oxide, nano cesium tungstate, nano ATO and nano ITO;
the transparent wood matrix comprises a delignified wood matrix and a high molecular polymer distributed in a pore structure of the delignified wood matrix, wherein the high molecular polymer is polymethyl methacrylate, epoxy resin or polydimethylsiloxane;
the preparation method of the transparent wood with the optical regulation and control function comprises the following steps of:
removing lignin in the wood matrix through chemical treatment, and then performing hydrophobic oleophylic modification treatment and drying treatment to obtain the lignin-removed wood matrix;
dispersing inorganic particles with an optical regulation function in a high molecular polymer monomer solution to obtain a dispersion liquid A, wherein the concentration of the inorganic particles in the dispersion liquid A is 0.01-0.1 wt%;
injecting the obtained dispersion liquid A into a delignified wood matrix, and then initiating a polymerization reaction of a high-molecular polymer monomer in the delignified wood matrix by ultraviolet irradiation or heating at 50-80 ℃ to obtain the transparent wood with the optical regulation function;
the chemical treatment is to place the wood substrate in a chemical reagent to react for 1-10 hours at 25-100 ℃, wherein the chemical reagent is at least one selected from hydrogen peroxide, a mixed solution of sodium hypochlorite and sodium hydroxide and perchloric acid;
the hydrophobic oleophylic modification treatment comprises the steps of immersing the chemically treated delignified wood matrix into a solution containing a modifier for reaction for 12-24 hours, wherein the concentration of the modifier in the solution containing the modifier is 0.01-0.1 mol/L, and the modifier is n-octadecanethiol, n-dodecanethiol or stearic acid;
the high molecular polymer monomer solution is methyl methacrylate solution, bisphenol A glycidyl ether solution or dimethyl siloxane solution;
the power of the ultraviolet illumination is 10-30W, and the time is 1-3 hours.
2. The method for preparing transparent wood with optical control function according to claim 1, wherein the injection method is a full cell method or a semi-limiting method.
3. The method for preparing transparent wood with optical control function as claimed in claim 1, wherein the concentration of inorganic particles in the dispersion liquid A is 0.03-0.1 wt%.
4. The method for preparing transparent wood with optical control function as claimed in claim 1, wherein the content of inorganic particles with optical control function in the transparent wood with optical control function is 0.03-0.04 wt%.
5. The method for preparing transparent wood with optical control function as claimed in claim 1, wherein the inorganic particles with optical control function have a grain size of 10-50 nm.
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| CN110900761B (en) * | 2019-11-26 | 2021-06-04 | 上海大学 | Transparent wood-based material containing element-doped vanadium dioxide nano powder and preparation method and application thereof |
| CN111702902A (en) * | 2020-06-24 | 2020-09-25 | 王怀远 | Preparation method of wood-based selective near-infrared absorbing material |
| CN112025888A (en) * | 2020-09-11 | 2020-12-04 | 浙江鹏远新材料科技集团股份有限公司 | Method for preparing transparent heat-insulating building material based on waste wood |
| CN115286931A (en) * | 2022-07-19 | 2022-11-04 | 深圳粤源建设有限责任公司 | Transparent wood, preparation method thereof and transparent furniture |
| CN115464734B (en) * | 2022-09-30 | 2023-06-20 | 西南民族大学 | Precursor solution, application thereof and preparation method of hydrophobic and low-moisture-absorption wood material |
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