CN112140264A - Transparent cellulose composite material and preparation method thereof - Google Patents
Transparent cellulose composite material and preparation method thereof Download PDFInfo
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- CN112140264A CN112140264A CN202011019100.0A CN202011019100A CN112140264A CN 112140264 A CN112140264 A CN 112140264A CN 202011019100 A CN202011019100 A CN 202011019100A CN 112140264 A CN112140264 A CN 112140264A
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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
- B27K3/025—Controlling the process
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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
- B27K3/005—Impregnating wood, e.g. impregnation pretreatment, for example puncturing; Wood impregnation aids not directly involved in the impregnation process employing compositions comprising microparticles
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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
- B27K3/007—Impregnating wood, e.g. impregnation pretreatment, for example puncturing; Wood impregnation aids not directly involved in the impregnation process employing compositions comprising nanoparticles
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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
- B27K3/16—Inorganic 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
- B27K3/16—Inorganic impregnating agents
- B27K3/22—Compounds of zinc or copper
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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
- B27K3/16—Inorganic impregnating agents
- B27K3/28—Compounds of arsenic or antimony
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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
- B27K3/16—Inorganic impregnating agents
- B27K3/32—Mixtures of different inorganic 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
- B27K3/34—Organic impregnating agents
- B27K3/38—Aromatic compounds
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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
- B27K3/34—Organic impregnating agents
- B27K3/38—Aromatic compounds
- B27K3/40—Aromatic compounds halogenated
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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
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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
- B27K5/003—Treating of wood not provided for in groups B27K1/00, B27K3/00 by using electromagnetic radiation or mechanical waves
- B27K5/0065—Ultrasonic treatment
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B27—WORKING OR PRESERVING WOOD OR SIMILAR MATERIAL; NAILING OR STAPLING MACHINES IN GENERAL
- B27N—MANUFACTURE BY DRY PROCESSES OF ARTICLES, WITH OR WITHOUT ORGANIC BINDING AGENTS, MADE FROM PARTICLES OR FIBRES CONSISTING OF WOOD OR OTHER LIGNOCELLULOSIC OR LIKE ORGANIC MATERIAL
- B27N1/00—Pretreatment of moulding material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B27—WORKING OR PRESERVING WOOD OR SIMILAR MATERIAL; NAILING OR STAPLING MACHINES IN GENERAL
- B27N—MANUFACTURE BY DRY PROCESSES OF ARTICLES, WITH OR WITHOUT ORGANIC BINDING AGENTS, MADE FROM PARTICLES OR FIBRES CONSISTING OF WOOD OR OTHER LIGNOCELLULOSIC OR LIKE ORGANIC MATERIAL
- B27N3/00—Manufacture of substantially flat articles, e.g. boards, from particles or fibres
- B27N3/08—Moulding or pressing
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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
- B27K2240/00—Purpose of the treatment
- B27K2240/15—Decontamination of previously treated wood
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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
- B27K2240/00—Purpose of the treatment
- B27K2240/90—UV-protection
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Abstract
The invention provides a transparent cellulose composite material, and a preparation method thereof comprises the steps of cutting, lignin removing, hemicellulose removing, fiber size refining, dispersion impregnation, curing molding and the like. The transparent cellulose composite material reserves a cellulose microporous structure, can be used for preparing finished products with any size after being soaked in polymer solution matched with the refractive index, is mixed with functional additives, and has optical selectivity. The transparent cellulose composite material has the advantages of good visible light band transmittance, excellent ultraviolet and near infrared ray resistance, small haze, arbitrary size, suitability for batch production and wide application value.
Description
Technical Field
The invention relates to the field of composite material preparation, in particular to a transparent cellulose composite material and a preparation method thereof.
Background
At present, social economy develops at a high speed, the living standard of people is gradually improved, and the serious environmental problems, such as pollution of air, soil and water resources, climate change, nondegradable garbage and the like, are accompanied. The sustainable development economy is in the forefront, and wood is an abundant organic high-molecular resource of the earth, is used as an environment-friendly and sustainable renewable material, and has good natural material properties including low density, high modulus, high strength, high toughness, low heat conduction coefficient, no toxicity, degradability and the like. The wood has special structure and chemical components due to the growth characteristics of the wood, and the wood has opacity. In recent years, researchers have used the paper pulp production process for reference to bleaching wood, and then pouring resin solution with similar refractive index to obtain transparent wood. The transparent wood is a light, heat-insulating and transparent composite material prepared by removing lignin and hemicellulose from wood and performing transparentization treatment, is further compounded with different nano particles, has optical selective permeability and good mechanical property, has potential application in a plurality of fields such as green building materials, LED lighting equipment, luminous magnetic switches, information storage, solar cells, anti-counterfeiting equipment and the like, and further replaces the use of traditional glass. However, the mechanical strength of the wood is greatly reduced along with the treatment process of the lignin, and the wood is not beneficial to maintaining the complete structure of the wood, so that the wood is only limited to laboratory research. It is important that an environmentally friendly material for wood applications replace traditional glass. With the development of urbanization and the living needs of people, about four to five thousand tons of waste glass are generated in China every year, and the complete degradation of the glass needs thousands of years. Since the waste glass is expensive in purification cost due to the influence of color, purity, etc., it is difficult to recycle the waste glass. Glass as a non-degradable waste material brings many potential insecurities to the soil and human life and production activities.
For example, the existing ultraviolet curing glue film glass is prepared by coating a layer of ultraviolet-resistant polymer coating on the surface of glass. The main body part of the technical scheme adopts the traditional glass material, so that the environmental protection property is poor. In addition, the scheme only has a certain function of blocking ultraviolet rays, and the heat insulation effect is poor.
For example, in the existing preparation method of the ultraviolet shielding transparent wood, the technical scheme is that wood slices are used for removing lignin and bleaching, then a PMMA resin solution is soaked, and the ultraviolet shielding transparent wood is obtained after curing, but the transparent wood prepared by the technical scheme has no shielding effect on near infrared rays.
Disclosure of Invention
Based on the above, in order to solve the problems of poor environmental protection, poor heat insulation effect and poor near infrared ray shielding effect of the conventional transparent material, the invention provides a preparation method of a transparent cellulose composite material, which comprises the following specific technical scheme:
a preparation method of a transparent cellulose composite material comprises the following steps:
cutting the collected wood;
soaking the cut wood in a lignin removal solution;
soaking the wood with the lignin removed in a hemicellulose removing liquid;
cleaning the wood without hemicellulose, and storing in a liquid seal manner;
crushing and thinning the cleaned wood;
adding the ultraviolet shielding additive and the near-infrared shielding additive into the polymer solution and uniformly mixing to obtain a composite solution;
impregnating and mixing the crushed and refined wood with the composite solution;
and (5) carrying out shaping and curing treatment by using a mould to obtain the transparent cellulose composite material.
According to the preparation method of the transparent cellulose composite material, lignin removal and hemicellulose removal treatment are carried out on wood, so that the content of lignin is less than 5%, the content of hemicellulose is less than 10%, and the microporous channel structure of cellulose is reserved; the wood fiber and the composite solution are impregnated and mixed, so that the structure of the cellulose is filled with the polymer solution, and the light transmittance of the obtained transparent cellulose composite material reaches 80%; by combining with functional additives, the composite material with the ultraviolet shielding rate of more than 99 percent and the near infrared shielding rate of more than 70 percent is obtained; the transparent cellulose composite material disclosed by the invention is high in visible light transmittance, can resist ultraviolet rays and near infrared rays, has the advantage of wide application scene, is environment-friendly in preparation process, is easier to degrade than the traditional glass material, and accords with sustainable development. The wood is used as a raw material, the material source is wide, the preparation process steps are simple, the wood can be made into any size, and the wood is suitable for large-scale production.
Further, the wood is selected from one or more of balsa, tung, pine and basswood, and the size of the cut wood is as follows: the length is 3cm-30cm, the width is 3cm-30cm, and the thickness is 5mm-10 mm.
Further, the lignin removal liquid is a mixed solution of strong alkali liquor, sulfite and bisulfite, the concentration of the strong alkali liquor is 0.5mol/L-5.0mol/L, and the concentrations of the sulfite and bisulfite are both 0.1mol/L-2.0 mol/L.
Further, the hemicellulose removing liquid is selected from hydrogen peroxide, hypochlorite or chlorite solution, and the mass percentage concentration is 5-35%.
Further, the cleaning is carried out by firstly adopting a weak acid aqueous solution under the ultrasonic condition, wherein the mass fraction of weak acid is 5-50%, and the cleaning time is 20-60 min; and then deionized water is adopted for cleaning for 3-5 times until the color of the deionized water is not changed, or the deionized water is soaked and boiled in heating boiling water for 12-48 hours until the color of the soaking and boiling water is not changed.
Further, the smashing and refining treatment comprises the steps of primarily grinding the cleaned wood, then treating the wood by using a TEMPO oxidation method under the condition of stirring, cleaning the treated wood particles, adjusting the pH value to be neutral by using hydrochloric acid with the mass fraction of 3% -10%, then smashing the wood particles to the size of 20nm-200nm by using a high-pressure homogenization method, and concentrating to obtain the smashed and refined wood.
Further, the ultraviolet and near infrared shielding additives comprise one or more of the following: nano zinc oxide particles, nano titanium dioxide particles, 2, 4-dihydroxy benzophenone, 2-hydroxy-4-methoxy benzophenone, 2-hydroxy-4-n-octoxy benzophenone, 2- (2-hydroxy-3, 5-di-tert-phenyl) -5-chlorinated benzotriazole, 2- (2-hydroxy-5-methylphenyl) benzotriazole, nano cesium tungsten bronze particles and nano tin antimony oxide particles.
Further, the impregnation and mixing of the wood after the pulverization and the thinning with the composite solution are as follows: based on the assistance of ultrasonic, mixing and impregnating the crushed and refined wood with a polymer solution by using stirring equipment, then vacuumizing to 200Pa, and treating for 0.5h-1h to obtain a mixed solution.
Further, the setting and curing treatment comprises the following steps: casting the composite solution in a mould with required size, curing for 10-30 h at the temperature of 20-70 ℃, and finally demoulding.
Further, the invention also provides a transparent cellulose composite material, and the composite material is prepared by adopting the preparation method.
Drawings
FIG. 1 is a photograph of a transparent cellulose composite prepared in example 1 of the present invention;
FIG. 2 is a graph showing the light transmittance results of the transparent cellulose composite prepared in example 1 of the present invention;
FIG. 3 is an SEM photograph of a transparent cellulose composite prepared in example 1 of the present invention;
FIG. 4 is a comparison of transmittance of the transparent cellulose composite prepared in example 1 of the present invention;
fig. 5 is a comparison result of the heat insulation effect of the transparent cellulose composite prepared in example 1 of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail below with reference to embodiments thereof. It should be understood that the detailed description and specific examples, while indicating the scope of the invention, are intended for purposes of illustration only and are not intended to limit the scope of the invention.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used herein in the description of the invention is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
The preparation method of the transparent cellulose composite material in one embodiment of the invention comprises the following steps:
s1, cutting the collected wood;
s2, soaking the cut wood in a lignin removal solution;
s3, soaking the wood subjected to lignin removal in a hemicellulose removal liquid;
s4, cleaning the wood without hemicellulose, and storing in a liquid seal manner;
s5, crushing and thinning the cleaned wood;
s6, adding the ultraviolet shielding additive and the near-infrared shielding additive into the polymer solution, and uniformly mixing to obtain a composite solution;
s7, dipping and mixing the crushed and refined wood and the composite solution;
and S8, carrying out shaping and curing treatment by using a mould to obtain the transparent cellulose composite material.
According to the preparation method of the transparent cellulose composite material, lignin removal and hemicellulose removal treatment are carried out on wood, so that the content of lignin is less than 5%, the content of hemicellulose is less than 10%, and the microporous channel structure of cellulose is reserved; the wood fiber and the composite solution are impregnated and mixed, so that the structure of the cellulose is filled with the polymer solution, and the light transmittance of the obtained transparent cellulose composite material reaches 80%; by combining with functional additives, the composite material with the ultraviolet shielding rate of more than 99 percent and the near infrared shielding rate of more than 70 percent is obtained; the transparent cellulose composite material disclosed by the invention is high in visible light transmittance, can resist ultraviolet rays and near infrared rays, has the advantage of wide application scene, is environment-friendly in preparation process, is easier to degrade than the traditional glass material, and accords with sustainable development. The wood is used as a raw material, the material source is wide, the preparation process steps are simple, the wood can be made into any size, and the wood is suitable for large-scale production.
In one embodiment, the wood is selected from one or more of balsa, tung, pine and basswood, and the cut wood has a size of: the length is 3cm-30cm, the width is 3cm-30cm, and the thickness is 5mm-10 mm.
In one embodiment, the lignin removal liquid is a mixed solution of strong alkali liquor, sulfite and bisulfite, the concentration of the strong alkali liquor is 0.5mol/L-5.0mol/L, and the concentrations of the sulfite and bisulfite are both 0.1mol/L-2.0 mol/L.
In one embodiment, the hemicellulose removal liquid is selected from hydrogen peroxide, hypochlorite or chlorite solutions, and the mass percentage concentration is 5% -35%.
In one embodiment, the cleaning is performed by firstly adopting a weak acid aqueous solution under an ultrasonic condition, the mass fraction of the weak acid is 5% -50%, and the cleaning time is 20-60 min; and then deionized water is adopted for cleaning for 3-5 times until the color of the deionized water is not changed, or the deionized water is soaked and boiled in heating boiling water for 12-48 hours until the color of the soaking and boiling water is not changed.
In one embodiment, the liquid seal is preserved by storing the cleaned wood in absolute ethyl alcohol.
In one embodiment, the smashing and refining treatment is to preliminarily grind the cleaned wood, then treat the cleaned wood by using a TEMPO oxidation method under the condition of stirring, after the treated wood particles are cleaned, use hydrochloric acid with the mass fraction of 3% -10% to adjust the pH value to be neutral, then smash the particle size of the wood particles to the size of 20nm-200nm by using a high-pressure homogenization method, and obtain the smashed and refined wood after concentration.
In one embodiment, the ultraviolet and near infrared shielding additives comprise one or more of the following: nano zinc oxide particles, nano titanium dioxide particles, 2, 4-dihydroxy benzophenone, 2-hydroxy-4-methoxy benzophenone, 2-hydroxy-4-n-octoxy benzophenone, 2- (2-hydroxy-3, 5-di-tert-phenyl) -5-chlorinated benzotriazole, 2- (2-hydroxy-5-methylphenyl) benzotriazole, nano cesium tungsten bronze particles and nano tin antimony oxide particles.
In one embodiment, the impregnation and mixing of the pulverized and refined wood and the composite solution are as follows: based on the assistance of ultrasonic, mixing and impregnating the crushed and refined wood with a polymer solution by using stirring equipment, then vacuumizing to 200Pa, and treating for 0.5h-1h to obtain a mixed solution.
Further, the stirring device is selected from: paddle mechanical stirrer, open turbine stirrer, propeller stirrer, long blade propeller stirrer, disc turbine stirrer, Brumakin stirrer and magnetic stirrer; the stirring conditions of the stirring device are 400-2000 rpm.
In one embodiment, the setting and curing process is as follows: casting the composite solution in a mould with required size, curing for 10-30 h at the temperature of 20-70 ℃, and finally demoulding.
In one embodiment, the soaking temperature in the lignin removal liquid is
The soaking time is 4-12 h at 80-100 ℃, so that the lignin content of the wood after soaking is less than 10%.
In one embodiment, the soaking temperature of the wood in the hemicellulose removing liquid is 80-100 ℃, and the soaking time is 4-12 hours, so that the hemicellulose content of the wood after soaking is less than 10%.
In one embodiment, the uv-screening additive and the near ir-screening additive are selected from one or more of the following components in parts by weight, based on 100 parts by weight of the polymer: 0.01-3.0 parts of nano zinc oxide particles; 0.01-5.0 parts of nano titanium dioxide particles; 0.01-2.0 parts of 2, 4-dihydroxy benzophenone; 0.02-2.0 parts of 2-hydroxy-4-methoxybenzophenone; 0.02-2.5 parts of 2-hydroxy-4-n-octoxy benzophenone; 0.01-1.5 parts of 2- (2-hydroxy-3, 5-di-tert-phenyl) -5-chlorobenzotriazole; 0.01-2.0 parts of 2- (2-hydroxy-5-methylphenyl) benzotriazole; 0.001-1.0 part of nano cesium tungsten bronze particles; 0.001-1.5 parts of nano tin antimony oxide particles.
In one embodiment, the polymer is a thermoplastic or thermoset polymer having a refractive index between 1.4 and 1.7, including but not limited to one of the following materials: polymethyl methacrylate, polyvinyl alcohol, epoxy resin, polycarbonate, polystyrene and polyvinylpyrrolidone.
In one embodiment, the transparent cellulose composite material is prepared by the preparation method.
Embodiments of the present invention will be described in detail below with reference to specific examples.
Example 1:
a preparation method of a transparent cellulose composite material comprises the following steps:
s1, cutting the tung wood into a plurality of test pieces of 80mm by 40mm by 5 mm;
s2, soaking the cut wood in a mixed solution of sodium hydroxide and sodium sulfite, wherein the concentration of the sodium hydroxide is 2.5mol/L, the concentration of the sodium sulfite is 0.4mol/L, the soaking temperature is 95 ℃, the soaking time is 8 hours, and the lignin content of the soaked wood is 5%;
s3, soaking the wood subjected to lignin removal in hydrogen peroxide, wherein the concentration of the hydrogen peroxide is 35%, the soaking temperature is 95 ℃, the soaking time is 10 hours, and the hemicellulose content of the soaked wood is 8%;
s4, in an ultrasonic cleaning machine, cleaning the wood without hemicellulose for 20min by using an acetic acid aqueous solution with the mass fraction of 5%, and then cleaning the wood for 5 times by using deionized water for 60min until the color of the deionized water is unchanged; and (3) soaking the cleaned wood in acetone/absolute ethyl alcohol to remove residual moisture, and finally, preserving the wood in a liquid seal mode by using absolute ethyl alcohol.
S5, primarily grinding the cleaned wood, treating the wood by using a TEMPO oxidation method under the condition of stirring, and after the wood is cleaned by deionized water, adjusting the pH value to 7 by using hydrochloric acid with the mass fraction of 5%; then, the particle size of the wood particles is crushed to 100nm by a high-pressure homogenization method, and the solution is concentrated to obtain the crushed and refined wood.
S6, weighing 3 parts by weight of nano zinc oxide particles, 0.5 part by weight of nano cesium tungsten bronze particles and 100 parts by weight of epoxy resin, and dispersing uniformly by using a mechanical stirrer under the condition of taking ultrasound as an auxiliary until no obvious particle agglomeration exists to obtain a composite solution.
S7, weighing 30 parts by weight of crushed and refined wood and 100 parts by weight of composite solution, dispersing uniformly by using a mechanical stirrer under the condition of taking ultrasound as an auxiliary condition until no obvious particles are agglomerated, then vacuumizing to 200Pa for treatment for 2 hours to completely soak the wood in the composite solution, and obtaining a mixed solution.
S8, casting the mixed solution in a mould with the size of 65mm multiplied by 5mm, curing for 20 hours at the temperature of 70 ℃, and finally performing demoulding treatment to obtain the transparent cellulose composite material.
The photograph of the transparent cellulose composite material prepared in this example is shown in FIG. 1, and the SEM photograph is shown in FIG. 3.
Example 2:
a preparation method of a transparent cellulose composite material comprises the following steps:
s1, cutting the balsawood into a plurality of test pieces of 80mm by 40mm by 5 mm;
s2, soaking the cut wood in a mixed solution of sodium hydroxide and sodium sulfite, wherein the concentration of the sodium hydroxide is 2.5mol/L, the concentration of the sodium sulfite is 0.4mol/L, the soaking temperature is 95 ℃, the soaking time is 8 hours, and the lignin content of the soaked wood is 3%;
s3, soaking the wood subjected to lignin removal in hydrogen peroxide, wherein the concentration of the hydrogen peroxide is 35%, the soaking temperature is 90 ℃, the soaking time is 10 hours, and the hemicellulose content of the soaked wood is 5%;
s4, in an ultrasonic cleaning machine, cleaning the wood without hemicellulose for 20min by using an acetic acid aqueous solution with the mass fraction of 5%, and then cleaning the wood for 4 times by using deionized water for 60min until the color of the deionized water is unchanged; and (3) soaking the cleaned wood in acetone/absolute ethyl alcohol to remove residual moisture, and finally, preserving the wood in a liquid seal mode by using absolute ethyl alcohol.
S5, primarily grinding the cleaned wood, treating the wood by using a TEMPO oxidation method under the condition of stirring, cleaning the wood by using deionized water, and adjusting the pH to 7 by using hydrochloric acid with the mass fraction of 5%; then, the particle size of the wood particles is crushed to 200nm by a high-pressure homogenization method, and the solution is concentrated to obtain the crushed and refined wood.
S6, weighing 1 part by weight of 2- (2-hydroxy-5-methylphenyl) benzotriazole, 0.1 part by weight of nano cesium tungsten bronze particles and 100 parts by weight of epoxy resin, and dispersing uniformly by using a mechanical stirrer under the condition of taking ultrasound as an auxiliary until no obvious particle agglomeration exists to obtain a composite solution.
S7, weighing 20 parts by weight of crushed and refined wood and 100 parts by weight of composite solution, dispersing uniformly by using a mechanical stirrer under the condition of taking ultrasound as an auxiliary condition until no obvious particles are agglomerated, then vacuumizing to 200Pa for treatment for 1h to completely soak the wood in the composite solution, and obtaining a mixed solution.
S8, casting the mixed solution in a mould with the size of 65mm multiplied by 5mm, curing for 30 hours at the temperature of 50 ℃, and finally demoulding to obtain the transparent cellulose composite material.
Example 3:
a preparation method of a transparent cellulose composite material comprises the following steps:
s1, cutting the tung wood into a plurality of test pieces of 80mm by 40mm by 5 mm;
s2, soaking the cut wood in a mixed solution of sodium hydroxide and sodium sulfite, wherein the concentration of the sodium hydroxide is 2.5mol/L, the concentration of the sodium sulfite is 0.4mol/L, the soaking temperature is 95 ℃, the soaking time is 8 hours, and the lignin content of the soaked wood is 5%;
s3, soaking the wood subjected to lignin removal in hydrogen peroxide, wherein the concentration of the hydrogen peroxide is 35%, the soaking temperature is 85 ℃, the soaking time is 10 hours, and the hemicellulose content of the soaked wood is 3%;
s4, in an ultrasonic cleaning machine, cleaning the wood without hemicellulose for 20min by using an acetic acid aqueous solution with the mass fraction of 5%, and then cleaning the wood for 3 times by using deionized water for 60min until the color of the deionized water is unchanged; and (3) soaking the cleaned wood in acetone/absolute ethyl alcohol to remove residual moisture, and finally, preserving the wood in a liquid seal mode by using absolute ethyl alcohol.
S5, primarily grinding the cleaned wood, treating the wood by using a TEMPO oxidation method under the condition of stirring, and after the wood is cleaned by deionized water, adjusting the pH value to 7 by using hydrochloric acid with the mass fraction of 8%; then, the particle size of the wood particles is crushed to 180nm by a high-pressure homogenization method, and the solution is concentrated to obtain the crushed and refined wood.
S6, weighing 2 parts by weight of nano zinc oxide particles, 0.8 part by weight of nano cesium tungsten bronze particles and 100 parts by weight of epoxy resin, and dispersing uniformly by using a mechanical stirrer under the condition of taking ultrasound as an auxiliary until no obvious particle agglomeration exists to obtain a composite solution.
S7, weighing 10 parts by weight of crushed and refined wood and 100 parts by weight of composite solution, dispersing uniformly by using a mechanical stirrer under the condition of taking ultrasound as an auxiliary condition until no obvious particles are agglomerated, then vacuumizing to 200Pa for treatment for 2 hours to completely soak the wood in the composite solution, and obtaining a mixed solution.
S8, casting the mixed solution in a mould with the size of 65mm multiplied by 5mm, curing for 10 hours at the temperature of 20 ℃, and finally performing demoulding treatment to obtain the transparent cellulose composite material.
In order to more clearly understand the effect of ultraviolet ray resistance and near infrared ray resistance prepared in the present application, the following comparative examples were also provided.
Comparative example 1:
the preparation method of the transparent cellulose composite material in the comparative example is as follows:
s1, cutting the balsawood into a plurality of test pieces of 80mm by 40mm by 5 mm;
s2, soaking the cut wood in a mixed solution of sodium hydroxide and sodium sulfite, wherein the concentration of the sodium hydroxide is 2.5mol/L, the concentration of the sodium sulfite is 0.4mol/L, the soaking temperature is 95 ℃, the soaking time is 8 hours, and the lignin content of the soaked wood is 1%;
s3, soaking the wood subjected to lignin removal in hydrogen peroxide, wherein the concentration of the hydrogen peroxide is 35%, the soaking temperature is 90 ℃, the soaking time is 10 hours, and the hemicellulose content of the soaked wood is 3%;
s4, in an ultrasonic cleaning machine, cleaning the wood without hemicellulose for 20mins by using an acetic acid aqueous solution with the mass fraction of 5%, and then cleaning the wood for 4 times by using deionized water for 60mins until the color of the deionized water is unchanged; and (3) soaking the cleaned wood in acetone/absolute ethyl alcohol to remove residual moisture, and finally, preserving the wood in a liquid seal mode by using absolute ethyl alcohol.
S5, primarily grinding the cleaned wood, treating the wood by using a TEMPO oxidation method under the condition of stirring, cleaning the wood by using deionized water, and adjusting the pH to 7 by using hydrochloric acid with the mass fraction of 5%; then, the particle size of the wood particles is crushed to 200nm by a high-pressure homogenization method, and the solution is concentrated to obtain the crushed and refined wood.
S6, weighing 20 parts by weight of crushed and refined wood and 100 parts by weight of epoxy resin, and dispersing uniformly by using a mechanical stirrer under the condition of taking ultrasound as an auxiliary until no obvious particle agglomeration exists. And vacuumizing the solution to 200Pa, and treating for 0.5-2 h to completely impregnate the wood with the epoxy resin to obtain a mixed solution.
S7, casting the mixed solution in a mould with the size of 65mm multiplied by 5mm, curing for 30 hours at the temperature of 50 ℃, and finally demoulding to obtain the transparent cellulose composite material.
Comparative example 2:
the preparation method of the transparent cellulose composite material in the comparative example is as follows:
s1, cutting the balsawood into a plurality of test pieces of 80mm by 40mm by 5 mm;
s2, soaking the cut wood in a mixed solution of sodium hydroxide and sodium sulfite, wherein the concentration of the sodium hydroxide is 2.5mol/L, the concentration of the sodium sulfite is 0.4mol/L, the soaking temperature is 95 ℃, the soaking time is 8 hours, and the lignin content of the soaked wood is 1%;
s3, soaking the wood subjected to lignin removal in hydrogen peroxide, wherein the concentration of the hydrogen peroxide is 35%, the soaking temperature is 90 ℃, the soaking time is 10 hours, and the hemicellulose content of the soaked wood is 3%;
s4, in an ultrasonic cleaning machine, cleaning the wood without hemicellulose for 20mins by using an acetic acid aqueous solution with the mass fraction of 5%, and then cleaning the wood for 4 times by using deionized water for 60mins until the color of the deionized water is unchanged; and (3) soaking the cleaned wood in acetone/absolute ethyl alcohol to remove residual moisture, and finally, preserving the wood in a liquid seal mode by using absolute ethyl alcohol.
S5, putting the cleaned wood into a container, adding epoxy resin according to the mass ratio of the wood to the epoxy resin of 1:5, vacuumizing to 200Pa, and treating for 0.5-2 h to completely impregnate the wood with the epoxy resin.
S6, taking out the impregnated wood, clamping the wood between two pieces of glass, curing for 10-30 hours at the temperature of 20-70 ℃, and finally demoulding and taking out to obtain the transparent cellulose composite material.
Comparative example 3:
as an example of conventional glass, flat glass for construction is commercially available.
Test example:
1. light transmittance test
The transparent cellulose composite material prepared in example 1 was subjected to a light transmittance test using a spectrophotometer, and the result is shown in fig. 2, which shows that the composite material prepared in example 1 has an ultraviolet ray shielding rate of 99% or more and a near infrared ray shielding rate of 70% or more.
The transmittance of the plate glass of comparative example 3, which was a conventional glass, was measured by the same spectrophotometer, and the transmittance results were compared with those of the transparent cellulose composite material prepared in example 1, as shown in FIG. 4. The results show that the transparent cellulose composite material prepared in example 1 of the present application has better shielding effects against ultraviolet rays and near infrared rays than the plate glass of comparative example 3.
The transparent cellulose composites prepared in examples 1 to 3, the transparent cellulose composites prepared in comparative examples 1 to 2, and comparative example 3 were subjected to light transmittance test analysis, and the results are shown in table 1.
Table 1:
as can be seen from the data analysis in table 1, the transparent cellulose composite prepared by the present application has excellent uv and near infrared ray resistance, which is significantly superior to the comparative sample randomly purchased on the market.
2. Haze test
Table 2 shows the haze results of the transparent cellulose composites prepared in examples 1-3, the transparent cellulose composites prepared in comparative examples 1-2, and comparative example 3 and other patent applications (publication No. CN110603124A), which are described in patent application publication No. CN110603124A, and comparative data analysis, which shows that the haze results of the transparent cellulose composites prepared in the present application are smaller than those of the products of comparative example 2 and the published patents.
Table 2:
3. tensile test
Table 3 shows that the transparent cellulose composites prepared in examples 1 to 3, the transparent cellulose composites prepared in comparative examples 1 to 2, and comparative example 3 have better mechanical properties than the respective comparative examples.
Table 3:
in combination, the ultraviolet shielding effect of the invention reaches 99%, the near infrared shielding effect reaches 70%, the visible light transmittance in the wavelength range of 380nm-780nm reaches 80%, and the haze is less than 25%. Therefore, the transparent cellulose composite material has good visible light band transmittance, excellent ultraviolet and near infrared ray resistance and small haze, can be manufactured into any size, is suitable for batch production, and has wide application value.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (10)
1. A preparation method of a transparent cellulose composite material is characterized by comprising the following steps:
cutting the collected wood;
soaking the cut wood in a lignin removal solution;
soaking the wood with the lignin removed in a hemicellulose removing liquid;
cleaning the wood without hemicellulose, and storing in a liquid seal manner;
crushing and thinning the cleaned wood;
adding the ultraviolet shielding additive and the near-infrared shielding additive into the polymer solution and uniformly mixing to obtain a composite solution;
impregnating and mixing the crushed and refined wood with the composite solution;
and (5) carrying out shaping and curing treatment by using a mould to obtain the transparent cellulose composite material.
2. The method for preparing a transparent cellulose composite according to claim 1, wherein the wood is selected from one or more of balsa, tung, pine and basswood, and the cut wood has a size of: the length is 3cm-30cm, the width is 3cm-30cm, and the thickness is 5mm-10 mm.
3. The method for preparing the transparent cellulose composite material according to claim 1, wherein the delignification solution is a mixed solution of strong alkali solution, sulfite and bisulfite, the concentration of the strong alkali solution is 0.5mol/L-5.0mol/L, and the concentrations of the sulfite and bisulfite are both 0.1mol/L-2.0 mol/L.
4. The preparation method of the transparent cellulose composite material according to claim 1, wherein the hemicellulose-removed liquid is selected from hydrogen peroxide, hypochlorite or chlorite solution, and the mass percentage concentration is 5-35%.
5. The preparation method of the transparent cellulose composite material according to claim 1, wherein the cleaning is performed by firstly using a weak acid aqueous solution under an ultrasonic condition, the mass fraction of the weak acid is 5-50%, and the cleaning time is 20-60 min; and then deionized water is adopted for cleaning for 3-5 times until the color of the deionized water is not changed, or the deionized water is soaked and boiled in heating boiling water for 12-48 hours until the color of the soaking and boiling water is not changed.
6. The preparation method of the transparent cellulose composite material as claimed in claim 1, wherein the pulverization and refinement treatment is to primarily grind the cleaned wood, then treat the wood by using a TEMPO oxidation method under stirring, clean the treated wood particles, adjust the pH value to be neutral by using hydrochloric acid with the mass fraction of 3% -10%, then pulverize the particle size of the wood particles to the size of 20nm-200nm by using a high-pressure homogenization method, and concentrate the pulverized and refined wood.
7. The method of preparing a transparent cellulosic composite according to claim 1, wherein the ultraviolet shielding additive and near infrared shielding additive comprise one or more of: nano zinc oxide particles, nano titanium dioxide particles, 2, 4-dihydroxy benzophenone, 2-hydroxy-4-methoxy benzophenone, 2-hydroxy-4-n-octoxy benzophenone, 2- (2-hydroxy-3, 5-di-tert-phenyl) -5-chlorinated benzotriazole, 2- (2-hydroxy-5-methylphenyl) benzotriazole, nano cesium tungsten bronze particles and nano tin antimony oxide particles.
8. The method for preparing a transparent cellulose composite material according to claim 1, wherein the impregnating and mixing of the pulverized and refined wood with the composite solution is: based on the assistance of ultrasonic, mixing and impregnating the crushed and refined wood with a polymer solution by using stirring equipment, then vacuumizing to 200Pa, and treating for 0.5h-1h to obtain a mixed solution.
9. The method for preparing a transparent cellulose composite material according to claim 1, wherein the setting and curing treatment is: casting the composite solution in a mould with required size, curing for 10-30 h at the temperature of 20-70 ℃, and finally demoulding.
10. A transparent cellulose composite material, characterized in that the composite material is prepared by the preparation method of any one of claims 1 to 9.
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