CN111702902A - Preparation method of wood-based selective near-infrared absorbing material - Google Patents

Preparation method of wood-based selective near-infrared absorbing material Download PDF

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Publication number
CN111702902A
CN111702902A CN202010585089.8A CN202010585089A CN111702902A CN 111702902 A CN111702902 A CN 111702902A CN 202010585089 A CN202010585089 A CN 202010585089A CN 111702902 A CN111702902 A CN 111702902A
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Prior art keywords
wood
infrared
absorbing material
based selective
tungsten
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CN202010585089.8A
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Chinese (zh)
Inventor
王怀远
陆袁威
王美琪
田雪峰
廖圆圆
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B27WORKING OR PRESERVING WOOD OR SIMILAR MATERIAL; NAILING OR STAPLING MACHINES IN GENERAL
    • B27KPROCESSES, 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
    • B27K5/00Treating of wood not provided for in groups B27K1/00, B27K3/00
    • B27K5/001Heating
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B27WORKING OR PRESERVING WOOD OR SIMILAR MATERIAL; NAILING OR STAPLING MACHINES IN GENERAL
    • B27KPROCESSES, 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
    • B27K3/00Impregnating wood, e.g. impregnation pretreatment, for example puncturing; Wood impregnation aids not directly involved in the impregnation process
    • B27K3/52Impregnating agents containing mixtures of inorganic and organic compounds
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B27WORKING OR PRESERVING WOOD OR SIMILAR MATERIAL; NAILING OR STAPLING MACHINES IN GENERAL
    • B27KPROCESSES, 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
    • B27K5/00Treating of wood not provided for in groups B27K1/00, B27K3/00
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B27WORKING OR PRESERVING WOOD OR SIMILAR MATERIAL; NAILING OR STAPLING MACHINES IN GENERAL
    • B27KPROCESSES, 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
    • B27K5/00Treating of wood not provided for in groups B27K1/00, B27K3/00
    • B27K5/04Combined bleaching or impregnating and drying of wood

Abstract

A preparation method of a wood-based selective near-infrared absorbing material belongs to the technical field of wood modification, and particularly relates to a preparation method of a transparent wood material. The invention aims to solve the problem that the existing transparent wood does not have the near-infrared absorption characteristic. The preparation method comprises the following steps: firstly, removing chromophoric groups to obtain a delignified wood substrate; secondly, preparing resin doped with near-infrared heat-absorbing materials; and thirdly, soaking the delignified wood substrate into the resin doped with the near-infrared heat-absorbing material, adding a curing agent and ethanol, performing vacuum permeation-pressure permeation cyclic treatment, and curing at normal pressure to obtain the wood-based selective near-infrared absorbing material. The advantages are that: firstly, the light transmittance can reach more than 85 percent, and the near infrared absorption rate exceeds 85 percent; secondly, the mechanical property of the wood is enhanced to a great extent, and the heat conductivity coefficient is only 0.175W/(m.K); thirdly, the cost is low, the process is simple and the preparation period is short. The method is mainly used for preparing the wood-based selective near-infrared absorption material.

Description

Preparation method of wood-based selective near-infrared absorbing material
Technical Field
The invention belongs to the technical field of wood modification, and particularly relates to a preparation method of a transparent wood material.
Background
The wood is a natural polymer material with high mechanical strength, low thermal conductivity and a plurality of micro-nano pore structures. The main chemical compositions of the cellulose-lignin composite material are cellulose, hemicellulose and lignin. At present, the research on the transparentization modification of wood at home and abroad is few, the problem of insufficient polymer permeation is generally solved by adopting single vacuum permeation or pressurization permeation, the cost is higher, the permeation effect is poorer, and the existing transparent wood does not have the near infrared absorption characteristic.
Disclosure of Invention
The invention aims to solve the problem that the existing transparent wood does not have the near-infrared absorption characteristic, and provides a preparation method of a wood-based selective near-infrared absorption material.
A preparation method of a wood-based selective near-infrared absorption material comprises the following steps:
firstly, removing chromophoric groups in wood to obtain a delignified wood substrate;
doping the metal tungsten organic chelate and the tungsten oxide nanowire serving as near-infrared absorbents into resin to obtain the resin doped with the near-infrared heat-absorbing material, wherein the mass fraction of the tungsten oxide nanowire in the resin doped with the near-infrared heat-absorbing material is 0.03-1%, and the mass fraction of the metal tungsten organic chelate in the resin doped with the near-infrared heat-absorbing material is 3-15%;
dipping the delignified wood substrate into resin doped with a near-infrared heat absorption material, adding a curing agent and ethanol, uniformly mixing, performing vacuum permeation-pressure permeation cyclic treatment for 1-2 h, and curing at normal pressure for 8-24 h to obtain a wood-based selective near-infrared absorption material; the single treatment of the vacuum infiltration-pressurization infiltration cyclic treatment comprises the following specific processes: vacuum infiltration is carried out for 5min under the vacuum pressure of 0.05 atm-0.1 atm, and then pressurized infiltration is carried out for 5min under the pressurizing pressure of 7 atm-8 atm; the volume ratio of the resin doped with the near-infrared heat-absorbing material to the curing agent is 3-4: 1; the volume ratio of the resin doped with the near-infrared heat-absorbing material to the ethanol is 90-100: 1.
The principle and the advantages of the invention are as follows: the wood-based selective near-infrared absorbing material prepared by the invention not only has high light transmittance (the light transmittance can reach more than 80%), but also has extremely strong near-infrared absorbing capacity (the near-infrared absorptivity exceeds 85%), and can capture a large amount of solar radiant heat; secondly, under the condition of keeping the original fiber structure of the wood, the invention fills the polymer with the refractive index similar to that of the cellulose, on one hand, the light transmittance of the wood can be improved, and simultaneously, the mechanical property and the heat preservation property of the wood are enhanced to a great extent, and the heat conductivity coefficient is only 0.175W/(m.K); the preparation method has the advantages of low cost, simple process and short preparation period, and can be used for commercial production and processing. The application of the composite material in the fields of energy-saving buildings and the like can play a good role in social value.
Detailed Description
The first embodiment is as follows: the embodiment is a preparation method of a wood-based selective near-infrared absorbing material, which is specifically completed according to the following steps:
firstly, removing chromophoric groups in wood to obtain a delignified wood substrate;
doping the metal tungsten organic chelate and the tungsten oxide nanowire serving as near-infrared absorbents into resin to obtain the resin doped with the near-infrared heat-absorbing material, wherein the mass fraction of the tungsten oxide nanowire in the resin doped with the near-infrared heat-absorbing material is 0.03-1%, and the mass fraction of the metal tungsten organic chelate in the resin doped with the near-infrared heat-absorbing material is 3-15%;
dipping the delignified wood substrate into resin doped with a near-infrared heat absorption material, adding a curing agent and ethanol, uniformly mixing, performing vacuum permeation-pressure permeation cyclic treatment for 1-2 h, and curing at normal pressure for 8-24 h to obtain a wood-based selective near-infrared absorption material; the single treatment of the vacuum infiltration-pressurization infiltration cyclic treatment comprises the following specific processes: vacuum infiltration is carried out for 5min under the vacuum pressure of 0.05 atm-0.1 atm, and then pressurized infiltration is carried out for 5min under the pressurizing pressure of 7 atm-8 atm; the volume ratio of the resin doped with the near-infrared heat-absorbing material to the curing agent is 3-4: 1; the volume ratio of the resin doped with the near-infrared heat-absorbing material to the ethanol is 90-100: 1.
The second embodiment is as follows: the present embodiment differs from the first embodiment in that: the specific process for removing the chromophoric group in the wood in the first step is as follows: firstly, drying a wood sheet at the temperature of 103-105 ℃ for 12-14 h to obtain a dried wood sheet; immersing the dried wood sheet into delignification solution, adjusting the pH of the delignification solution to 4-5 by using glacial acetic acid, and then treating for 8-12 h at the water bath temperature of 75-95 ℃ to obtain treated wood; the delignification solution is a sodium chlorite solution with the mass fraction of 2.5-3.5%; bleaching the treated wood by adopting hydrogen peroxide with the mass fraction of 7-25% to obtain bleached wood; fourthly, the bleached wood is washed by deionized water for 10s to 30s, and then extracted and dehydrated by a dehydrating agent to obtain the delignified wood substrate. The rest is the same as the first embodiment.
Third embodiment the present embodiment is different from the second embodiment in that the wood sheet is made of basswood and has a density of 500kg/m at step ①3~550kg/m3. The rest is the same as the second embodiment.
The fourth concrete implementation mode: the present embodiment differs from the second or third embodiment in that: the dehydrating agent in the step I is a mixed solution of ethanol and acetone, and is formed by mixing acetone and 99.5% ethanol in a volume ratio of 1: 1. The other embodiments are the same as the second or third embodiment.
The fifth concrete implementation mode: the difference between this embodiment and one of the first to fourth embodiments is: the metal tungsten organic chelate in the second step is prepared by the following steps: uniformly mixing tungsten hexachloride and tributyl phosphate, and then heating and stirring at the temperature of 75-85 ℃ to react for 15-20 min to obtain a metal tungsten organic chelate; the volume ratio of the mass of the tungsten hexachloride to the tributyl phosphate is 1g:100 mL. The rest is the same as the first to fourth embodiments.
The sixth specific implementation mode: the difference between this embodiment and one of the first to fifth embodiments is as follows: the tungsten oxide nanowire in the second step is prepared according to the following steps: putting tungsten hexachloride into absolute ethyl alcohol, and then putting the tungsten hexachloride into high pressure reactionReacting for 10 to 15 hours in a kettle at the temperature of 180 ℃ to obtain the tungsten oxide nanowire with the chemical formula of WO2.72(ii) a The volume ratio of the mass of the tungsten hexachloride to the absolute ethyl alcohol is (0.1-0.12) g:20 mL. The rest is the same as the first to fifth embodiments.
The seventh embodiment: the difference between this embodiment and one of the first to sixth embodiments is: and in the second step, the particle size of the tungsten oxide nanowire is 20-40 nm. The rest is the same as the first to sixth embodiments.
The specific implementation mode is eight: the difference between this embodiment and one of the first to seventh embodiments is: in the second step, the resin is a composite resin of benzyl alcohol, a homopolymer of 2, 2' - [ (1-methylethylidene) bis (4, 1-phenylene formaldehyde) ] diepoxy ethane or alpha- (2-aminomethyl ethyl) -omega- (2-aminomethyl ethoxy) poly [ oxy (methyl-1, 2-ethylene) ]. The rest is the same as the first to seventh embodiments.
The invention is not limited to the above embodiments, and one or a combination of several embodiments may also achieve the object of the invention.
The following tests were carried out to confirm the effects of the present invention
Example 1: a preparation method of a wood-based selective near-infrared absorption material comprises the following steps:
firstly, removing chromophoric groups in wood to obtain a delignified wood substrate;
doping the metal tungsten organic chelate and the tungsten oxide nanowires into resin as near-infrared absorbent to obtain the resin doped with the near-infrared heat-absorbing material, wherein the mass fraction of the tungsten oxide nanowires in the resin doped with the near-infrared heat-absorbing material is 2.5%, and the mass fraction of the metal tungsten organic chelate in the resin doped with the near-infrared heat-absorbing material is 15%;
dipping the delignified wood substrate into resin doped with a near-infrared heat absorption material, adding a curing agent and ethanol, uniformly mixing, performing vacuum permeation-pressure permeation cyclic treatment for 1 hour, and curing for 8 hours at normal pressure to obtain a wood-based selective near-infrared absorption material; the specific process of the single treatment of the vacuum infiltration-pressurization infiltration cyclic treatment is as follows: vacuum infiltrating under vacuum pressure of 0.07atm for 5min, and then pressurizing and infiltrating under pressurizing pressure of 7.5atm for 5 min; the volume ratio of the resin doped with the near-infrared heat-absorbing material to the curing agent is 3.5: 1; the volume ratio of the resin doped with the near-infrared heat-absorbing material to the ethanol is 95: 1.
The specific process for removing chromophoric groups in the wood in the first implementation step is that ①, the wood sheet is dried for 12 hours at the temperature of 103 ℃ to obtain the dried wood sheet, the wood sheet is made of basswood and has the density of 515.4kg/m3②, immersing a dried wood thin plate into a delignification solution, adjusting the pH value of the delignification solution to 4.6 by using glacial acetic acid, then treating at 85 ℃ in a water bath for 11 hours to obtain treated wood, wherein the delignification solution is a sodium chlorite solution with the mass fraction of 3.0%, ③ is used for bleaching the treated wood by using hydrogen peroxide with the mass fraction of 7% to obtain bleached wood, ④ is used for washing the bleached wood for 10 seconds by using deionized water, and then extracting and dehydrating by using a dehydrating agent to obtain the delignified wood substrate, the dehydrating agent is a mixed solution of ethanol and acetone, and the dehydrating agent is formed by mixing the acetone and the ethanol with the mass fraction of 99.5% according to the volume ratio of 1: 1.
The metal tungsten organic chelate in the second implementation step is prepared by the following steps: uniformly mixing tungsten hexachloride and tributyl phosphate, and then heating, stirring and reacting at 80 ℃ for 15min to obtain a metal tungsten organic chelate; the volume ratio of the mass of the tungsten hexachloride to the tributyl phosphate is 1g:100 mL.
The tungsten oxide nanowire in the second implementation step is prepared according to the following steps: putting tungsten hexachloride into absolute ethyl alcohol, then putting the absolute ethyl alcohol into a high-pressure reaction kettle, and reacting for 12 hours at the temperature of 180 ℃ to obtain tungsten oxide nanowires, wherein the chemical formula of the tungsten oxide nanowires is WO2.72(ii) a The volume ratio of the mass of the tungsten hexachloride to the absolute ethyl alcohol is 0.1g:20 mL; the particle size of the tungsten oxide nano wire is 20 nm-40 nm.
In the second embodiment, the resin is a homopolymer of 2, 2' - [ (1-methylethylidene) bis (4, 1-phenylene carbaldehyde) ] bisoxirane.
The detection of the visible light transmittance of the wood-based selective near-infrared absorbing material obtained in example 1 shows that the visible light transmittance is 80%
The wood-based selective near-infrared absorption material obtained in example 1 was subjected to near-infrared absorption rate detection, and it was found that the near-infrared absorption rate was 85%
The thermal conductivity of the wood-based selective near-infrared absorbing material obtained in example 1 was measured, and it was found that the thermal conductivity was 0.175W/(m · K).

Claims (8)

1. The preparation method of the wood-based selective near-infrared absorption material is characterized by comprising the following steps of:
firstly, removing chromophoric groups in wood to obtain a delignified wood substrate;
doping the metal tungsten organic chelate and the tungsten oxide nanowire serving as near-infrared absorbents into resin to obtain the resin doped with the near-infrared heat-absorbing material, wherein the mass fraction of the tungsten oxide nanowire in the resin doped with the near-infrared heat-absorbing material is 0.03-1%, and the mass fraction of the metal tungsten organic chelate in the resin doped with the near-infrared heat-absorbing material is 3-15%;
dipping the delignified wood substrate into resin doped with a near-infrared heat absorption material, adding a curing agent and ethanol, uniformly mixing, performing vacuum permeation-pressure permeation cyclic treatment for 1-2 h, and curing at normal pressure for 8-24 h to obtain a wood-based selective near-infrared absorption material; the single treatment of the vacuum infiltration-pressurization infiltration cyclic treatment comprises the following specific processes: vacuum infiltration is carried out for 5min under the vacuum pressure of 0.05 atm-0.1 atm, and then pressurized infiltration is carried out for 5min under the pressurizing pressure of 7 atm-8 atm; the volume ratio of the resin doped with the near-infrared heat-absorbing material to the curing agent is 3-4: 1; the volume ratio of the resin doped with the near-infrared heat-absorbing material to the ethanol is 90-100: 1.
2. The method for preparing a wood-based selective near infrared absorbing material according to claim 1, wherein the specific process for removing chromophoric groups in wood in the first step is as follows: firstly, drying a wood sheet at the temperature of 103-105 ℃ for 12-14 h to obtain a dried wood sheet; immersing the dried wood sheet into delignification solution, adjusting the pH of the delignification solution to 4-5 by using glacial acetic acid, and then treating for 8-12 h at the water bath temperature of 75-95 ℃ to obtain treated wood; the delignification solution is a sodium chlorite solution with the mass fraction of 2.5-3.5%; bleaching the treated wood by adopting hydrogen peroxide with the mass fraction of 7-25% to obtain bleached wood; fourthly, the bleached wood is washed by deionized water for 10s to 30s, and then extracted and dehydrated by a dehydrating agent to obtain the delignified wood substrate.
3. The method of claim 2, wherein the wood sheet is basswood in the step ①, and the density of the wood sheet is 500kg/m3~550kg/m3
4. The method for preparing a wood-based selective near-infrared absorbing material according to claim 2 or 3, wherein the dehydrating agent in step (i) is a mixed solution of ethanol and acetone, and is prepared by mixing acetone and 99.5% by mass of ethanol in a volume ratio of 1: 1.
5. The method of claim 1, wherein the metal tungsten organic chelate in step two is prepared by the following steps: uniformly mixing tungsten hexachloride and tributyl phosphate, and then heating and stirring at the temperature of 75-85 ℃ to react for 15-20 min to obtain a metal tungsten organic chelate; the volume ratio of the mass of the tungsten hexachloride to the tributyl phosphate is 1g:100 mL.
6. The method for preparing the wood-based selective near infrared absorption material according to claim 1 or 5, wherein the tungsten oxide nanowires in the second step are prepared by the following steps: putting tungsten hexachloride into absolute ethyl alcohol, and then putting the tungsten hexachloride at high temperatureReacting for 10 to 15 hours in a pressure reaction kettle at the temperature of 180 ℃ to obtain the tungsten oxide nanowire with the chemical formula of WO2.72(ii) a The volume ratio of the mass of the tungsten hexachloride to the absolute ethyl alcohol is (0.1-0.12) g:20 mL.
7. The method for preparing the wood-based selective near infrared absorption material according to claim 1 or 6, wherein the particle size of the tungsten oxide nanowires in the second step is 20nm to 40 nm.
8. The method of claim 1, wherein in step two the resin is a benzyl alcohol-based composite resin, a homopolymer of 2, 2' - [ (1-methylethylene) bis (4, 1-phenylethanecarboxaldehyde) ] dioxirane, or a- (2-aminomethylethyl) - ω - (2-aminomethylethoxy) poly [ oxy (methyl-1, 2-ethylene) ].
CN202010585089.8A 2020-06-24 2020-06-24 Preparation method of wood-based selective near-infrared absorbing material Withdrawn CN111702902A (en)

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2009073117A (en) * 2007-09-21 2009-04-09 Iida Kogyo Kk Surface processing method of woody material
CN103539205A (en) * 2013-11-15 2014-01-29 哈尔滨工业大学 Method for preparing controllable-morphology-and-size mixed-valence tungsten-based nanoparticles
CN108527572A (en) * 2017-03-06 2018-09-14 上海大学 A kind of transparent wood and preparation method thereof with optics adjusting function
CN109971134A (en) * 2014-06-11 2019-07-05 亿高应用材料有限公司 Near infrared light screened film and its manufacturing method
CN110154183A (en) * 2019-06-14 2019-08-23 陕西科技大学 A kind of preparation method of ultraviolet shielded transparent timber
CN110304659A (en) * 2019-07-22 2019-10-08 广东工业大学 A kind of WO3Nano wire and the preparation method and application thereof

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2009073117A (en) * 2007-09-21 2009-04-09 Iida Kogyo Kk Surface processing method of woody material
CN103539205A (en) * 2013-11-15 2014-01-29 哈尔滨工业大学 Method for preparing controllable-morphology-and-size mixed-valence tungsten-based nanoparticles
CN109971134A (en) * 2014-06-11 2019-07-05 亿高应用材料有限公司 Near infrared light screened film and its manufacturing method
CN108527572A (en) * 2017-03-06 2018-09-14 上海大学 A kind of transparent wood and preparation method thereof with optics adjusting function
CN110154183A (en) * 2019-06-14 2019-08-23 陕西科技大学 A kind of preparation method of ultraviolet shielded transparent timber
CN110304659A (en) * 2019-07-22 2019-10-08 广东工业大学 A kind of WO3Nano wire and the preparation method and application thereof

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Application publication date: 20200925