CN108145816A - A kind of method of wood surface growth in situ nano-Ag particles - Google Patents

A kind of method of wood surface growth in situ nano-Ag particles Download PDF

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Publication number
CN108145816A
CN108145816A CN201711405429.9A CN201711405429A CN108145816A CN 108145816 A CN108145816 A CN 108145816A CN 201711405429 A CN201711405429 A CN 201711405429A CN 108145816 A CN108145816 A CN 108145816A
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China
Prior art keywords
timber
wood surface
surface growth
nano
particles
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Pending
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CN201711405429.9A
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Chinese (zh)
Inventor
李坚
高汝楠
肖少良
甘文涛
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Northeast Forestry University
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Northeast Forestry University
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Priority to CN201711405429.9A priority Critical patent/CN108145816A/en
Publication of CN108145816A publication Critical patent/CN108145816A/en
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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
    • 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
    • B27K3/00Impregnating wood, e.g. impregnation pretreatment, for example puncturing; Wood impregnation aids not directly involved in the impregnation process
    • B27K3/16Inorganic impregnating agents
    • 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

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  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Wood Science & Technology (AREA)
  • Forests & Forestry (AREA)
  • Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical And Physical Treatments For Wood And The Like (AREA)

Abstract

A kind of method of wood surface growth in situ nano-Ag particles, the present invention relates to the methods of wood surface growth Argent grain.The problem of the invention solves the prior arts to exist in wood surface growth in situ nano-Ag particles, and reagent is toxic, high energy consumption.Preparation method:First, timber is immersed in Tris buffer solutions, magnetic agitation, then Dopamine hydrochloride is added in into the Tris buffer solutions for being soaked with timber, mixture is obtained, is stirred at room temperature, takes out timber, then the timber taken out is cleaned with deionized water, vacuum drying, obtaining load has the timber of poly-dopamine coating;2nd, the timber that load has poly-dopamine coating is immersed in containing Ag+Solution in, stir at room temperature, take out timber, then with deionized water clean take out timber, vacuum drying, obtain surface in situ grow nano-Ag particles timber.The present invention is used for a kind of method of wood surface growth in situ nano-Ag particles.

Description

A kind of method of wood surface growth in situ nano-Ag particles
Technical field
The present invention relates to the methods of wood surface growth Argent grain.
Background technology
Timber be a kind of rich reserves, intensity it is high, it is biodegradable, can bio-compatible sustainable development material.Timber Conventional use penetrate into the every aspect of daily life already, such as furniture, artifacts, paper products and medical supplies.But Timber is developed into functional high-tech forward position material urgently to explore.It in recent years, will be inorganic with the rise of nanometer technology Nanomaterial loadings prepare functional inorganic nano/Wood composite material and have received widespread attention in wood surface, and by This has drawn a large amount of research.In existing common method of modifying, exist need to pre-process wood surface, reagent it is toxic And the defects of high energy consumption, limit the functional modification of timber.For example, wood surface is modified using chemical plating method When, it needs in advance to carry out wood surface activation introducing active centre, subsequent plating process could be carried out.This chemical plating outside Method is related to the toxic chemicals such as formaldehyde, stannous chloride.Inorganic nano/Wood composite material prepared by hydro-thermal method needs high temperature Treatment conditions such as (150 DEG C~200 DEG C), increase energy consumption.
The non-specific antibacterial characteristics of metallic silver, particularly nano silver are widely used in medical field always.With bulk Silver is compared, and nano silver has the specific surface area of bigger, therefore with better anti-microbial property.Develop it is simple and practicable, it is environmentally protective Method Ag is anchored on wood surface in situ, prepare the composite wooden material with anti-microbial property and use model to widen timber It encloses, the added value for improving timber has a very important significance.
In conclusion the prior art exists in wood surface growth in situ nano-Ag particles, reagent is toxic, high energy consumption Problem.
Invention content
The invention solves the prior arts to exist in wood surface growth in situ nano-Ag particles, and reagent is toxic, energy consumption The problem of high, and a kind of method of wood surface growth in situ nano-Ag particles is provided.
A kind of method of wood surface growth in situ nano-Ag particles follows the steps below:
First, timber is immersed in Tris buffer solutions, magnetic agitation 10min~30min, then is buffered to the Tris for being soaked with timber Dopamine hydrochloride is added in liquid, obtains mixture, 2h~for 24 hours is stirred at room temperature, timber is taken out, then cleans taking-up with deionized water Timber, and in temperature under conditions of 20 DEG C~150 DEG C, to be dried in vacuo 1h~48h, obtaining load has poly-dopamine coating Timber;
The Tris pH of buffer is 7.5~8.5;A concentration of 0.5mg/mL of Dopamine hydrochloride in the mixture~ 5mg/mL;
2nd, the timber that load has poly-dopamine coating is immersed in containing Ag+Solution in, at room temperature stir 30min~ 36h takes out timber, the timber taken out is then cleaned with deionized water, and under conditions of temperature is 40 DEG C~150 DEG C, vacuum Dry 1h~48h obtains the timber of surface in situ growth nano-Ag particles;
Described contains Ag+Solution in Ag+A concentration of 1 × 10-3Mol/L~1mol/L.
The beneficial effects of the invention are as follows:During loading nano silvery particle, without being pre-processed to timber;It is nontoxic using reagent And with biocompatibility;In addition to desiccated wood, reaction carries out under room temperature (25 DEG C or so), and low energy consumption, nano-Ag particles Load efficiency is high, and load factor reaches more than 95%.
The present invention is used for a kind of method of wood surface growth in situ nano-Ag particles.
Description of the drawings
Fig. 1 is the scanning electron microscope (SEM) photograph of poplar described in one step 1 of embodiment;
Fig. 2 is the timber low power scanning electron microscope (SEM) photograph that surface in situ prepared by embodiment one grows nano-Ag particles;
Fig. 3 is the timber high power scanning electron microscope (SEM) photograph that surface in situ prepared by embodiment one grows nano-Ag particles;
Fig. 4 is X ray diffracting spectrum, and a is the poplar described in two step 1 of embodiment, and b is table prepared by embodiment two The timber of face growth in situ nano-Ag particles;
Fig. 5 is the timber antibacterial experiment figure that surface in situ prepared by embodiment two grows nano-Ag particles.
Specific embodiment
Technical solution of the present invention is not limited to the specific embodiment of act set forth below, further include each specific embodiment it Between arbitrary combination.
Specific embodiment one:A kind of method of wood surface growth in situ nano-Ag particles described in present embodiment is It follows the steps below:
First, timber is immersed in Tris buffer solutions, magnetic agitation 10min~30min, then is buffered to the Tris for being soaked with timber Dopamine hydrochloride is added in liquid, obtains mixture, 2h~for 24 hours is stirred at room temperature, timber is taken out, then cleans taking-up with deionized water Timber, and in temperature under conditions of 20 DEG C~150 DEG C, to be dried in vacuo 1h~48h, obtaining load has poly-dopamine coating Timber;
The Tris pH of buffer is 7.5~8.5;A concentration of 0.5mg/mL of Dopamine hydrochloride in the mixture~ 5mg/mL;
2nd, the timber that load has poly-dopamine coating is immersed in containing Ag+Solution in, at room temperature stir 30min~ 36h takes out timber, the timber taken out is then cleaned with deionized water, and under conditions of temperature is 40 DEG C~150 DEG C, vacuum Dry 1h~48h obtains the timber of surface in situ growth nano-Ag particles;
Described contains Ag+Solution in Ag+A concentration of 1 × 10-3Mol/L~1mol/L.
The advantageous effect of present embodiment is:During loading nano silvery particle, without being pre-processed to timber;Using reagent It is nontoxic and with biocompatibility;In addition to desiccated wood, reaction carries out under room temperature (25 DEG C or so), and low energy consumption, nano silver Particulate load is efficient, and load factor reaches more than 95%.
Specific embodiment two:The present embodiment is different from the first embodiment in that:Timber described in step 1 For softwood or broadleaf.It is other same as the specific embodiment one.
Specific embodiment three:Unlike one of present embodiment and specific embodiment one or two:Institute in step 2 That states contains Ag+Solution be silver nitrate solution or silver ammino solution.It is other the same as one or two specific embodiments.
Specific embodiment four:Unlike one of present embodiment and specific embodiment one to three:In step 1 so The timber taken out is cleaned with deionized water afterwards, and under conditions of temperature is 60 DEG C~150 DEG C, is dried in vacuo 1h~48h.It is other It is identical with specific embodiment one to three.
Specific embodiment five:Unlike one of present embodiment and specific embodiment one to four:Institute in step 1 A concentration of 1mg/mL~2mg/mL of Dopamine hydrochloride in the mixture stated.It is other identical with specific embodiment one to four.
Specific embodiment six:Unlike one of present embodiment and specific embodiment one to five:It will in step 2 The timber that loading has poly-dopamine coating is immersed in containing Ag+Solution in, stir 1h~for 24 hours at room temperature.Other and specific reality It is identical to apply mode one to five.
Specific embodiment seven:Unlike one of present embodiment and specific embodiment one to six:Institute in step 2 That states contains Ag+Solution in Ag+A concentration of 0.5 × 10-3Mol/L~0.5 × 10-2mol/L.Other and specific embodiment One to six is identical.
Specific embodiment eight:Unlike one of present embodiment and specific embodiment one to seven:Institute in step 2 That states contains Ag+Solution in Ag+A concentration of 5 × 10-2mol/L.It is other identical with specific embodiment one to seven.
Specific embodiment nine:Unlike one of present embodiment and specific embodiment one to eight:Institute in step 2 That states contains Ag+Solution in Ag+A concentration of 0.5mol/L.It is other identical with specific embodiment one to eight.
Specific embodiment ten:Unlike one of present embodiment and specific embodiment one to nine:In step 2 so The timber taken out is cleaned with deionized water afterwards, and under conditions of temperature is 60 DEG C~150 DEG C, is dried in vacuo 1h~48h.It is other It is identical with specific embodiment one to nine.
Beneficial effects of the present invention are verified using following embodiment:
Embodiment one:
A kind of method of wood surface growth in situ nano-Ag particles follows the steps below:
First, timber is immersed in Tris buffer solutions, magnetic agitation 30min, then added into the Tris buffer solutions for be soaked with timber Enter Dopamine hydrochloride, obtain mixture, be stirred at room temperature for 24 hours, take out timber, the timber taken out is then cleaned with deionized water, and Under conditions of temperature is 60 DEG C, 6h is dried in vacuo, obtaining load has the timber of poly-dopamine coating;
The Tris pH of buffer is 8.5;A concentration of 0.5mg/mL of Dopamine hydrochloride in the mixture;
2nd, the timber that load has poly-dopamine coating is immersed in containing Ag+Solution in, stir 3h at room temperature, take out Then timber cleans the timber taken out with deionized water, and under conditions of temperature is 60 DEG C, is dried in vacuo 12h, obtains surface The timber of growth in situ nano-Ag particles;
Described contains Ag+Solution in Ag+A concentration of 5 × 10-2mol/L。
Timber described in step 1 is poplar;
Contain Ag described in step 2+Solution be silver ammino solution.
Fig. 1 is the scanning electron microscope (SEM) photograph of poplar described in one step 1 of embodiment;Fig. 2 is surface in situ prepared by embodiment one Grow the timber low power scanning electron microscope (SEM) photograph of nano-Ag particles;Fig. 3 is that surface in situ prepared by embodiment one grows nano-Ag particles Timber high power scanning electron microscope (SEM) photograph, as seen from the figure spherical nano-Ag particles be successfully grown in wood surface.
The present embodiment nano-Ag particles load efficiency is high, and load factor reaches 95%.
Embodiment two:
A kind of method of wood surface growth in situ nano-Ag particles follows the steps below:
First, timber is immersed in Tris buffer solutions, magnetic agitation 30min, then added into the Tris buffer solutions for be soaked with timber Enter Dopamine hydrochloride, obtain mixture, be stirred at room temperature 3h, take out timber, then clean the timber of taking-up with deionized water, and Under conditions of temperature is 45 DEG C, for 24 hours, obtaining load has the timber of poly-dopamine coating for vacuum drying;
The Tris pH of buffer is 8.5;A concentration of 2mg/mL of Dopamine hydrochloride in the mixture;
2nd, the timber that load has poly-dopamine coating is immersed in containing Ag+Solution in, stir at room temperature for 24 hours, take out Then timber cleans the timber taken out with deionized water, and under conditions of temperature is 45 DEG C, is dried in vacuo 48h, obtains surface The timber of growth in situ nano-Ag particles;
Described contains Ag+Solution in Ag+A concentration of 0.5mol/L;
Timber described in step 1 is poplar;
Contain Ag described in step 2+Solution be silver nitrate solution.
Fig. 4 is X ray diffracting spectrum, and a is the poplar described in two step 1 of embodiment, and b is table prepared by embodiment two The timber of face growth in situ nano-Ag particles;As seen from the figure, in addition to the characteristic peak of poplar also has the characteristic peak of silver, it was demonstrated that nanometer Silver is successfully loaded wood surface.
Fig. 5 is that the surface in situ of preparation prepared by embodiment two grows the timber antibacterial experiment figure of nano-Ag particles, antibacterial What experiment specifically carried out according to the following steps:A diameter of 10mm first is made in the timber of surface in situ growth nano-Ag particles first And the sequin that thickness is 1mm, sequin are used to do antibacterial experiment.
1st, culture medium is configured:
By 3 grams of beef extracts, 10 grams of peptones, 5 grams of NaCl are added in beaker, then 1000 milliliters of distillations are added into beaker Water obtains mixed liquor, and mixed liquor acid-base value is adjusted to 7.2 with NaOH solution, and is heated to mixed liquor and generates minute bubbles, then by fine jade Fat item is added in mixed liquor and stirs evenly, and is heated to agar strip and is completely dissolved, obtains culture medium, the culture medium that will be configured It is divided in conical flask, tampon, which is made, with degreasing cotton blocks taper bottleneck, and with rope and brown paper by the cone equipped with culture medium Shape bottle closure.Culture medium in conical flask is poured into clean small test tube (a quarter of liquid level to test tube to three/ One), with degreasing cotton be made tampon block test tube mouth and with rope and brown paper by equipped with culture medium test tube seal.After sealing Conical flask after test tube and sealing is placed in high-pressure sterilizing pot, after boosting to 0.1MPa, under conditions of pressure is 0.1MPa, is protected It holds 30 minutes.After open high-pressure sterilizing pot and take out the test tube after sealing and the conical flask after sealing.Test tube is put Cool down on inclined-plane, be inoculated on a sterile work bench after its cooled and solidified.
2nd, it is inoculated with:
Aseptic experiment platform switch is opened, first being sterilized 5 minutes or so with ultraviolet lamp (needs before operation with alcohol cotton rub hand and work Platform).Alcolhol burner is lighted, all operations are both needed to carry out close to flame vicinity, to prevent contaminating some other miscellaneous bacterias during operation. Transfer needle is burnt on flame red, strain and culture medium are opened in flame vicinity, with transfer needle under stroke is several in strain, and Curve stroke in the culture medium of test tube, is sealed and the number of patch with rubber stopper.Test tube after inoculation is put into 28.0 degrees Celsius of constant temperature Start to cultivate in incubator, further take out after 24 hours.
The strain is the Escherichia coli ATCC25922 of purchase.
3rd, bacteria suspension is prepared:
Physiological saline is first prepared first, and after volumetric flask constant volume, 10 milliliters of physiological saline are pipetted into mark with pipette Have in stoste test tube, dilution (10 is indicated with 6 pipetting 9 milliliters respectively-1、10-2、10-3、10-4、10-5、10-6) test tube In.And the fine taper bottle equipped with several beades and the small test tube equipped with physiological saline are put into sterilizing 30 inside high-pressure sterilizing pot Minute.
10 milliliters of stostes are poured into the small test tube for filling strain, shake and scrape off the bacterium that is attached on culture medium with acicula is connect Kind, it pours into fine taper bottle, strain is smashed and shakes up bacterium by the small bead shaken inside conical flask.It is moved with liquid-transfering gun 1 milliliter of bacterium solution is taken to be designated as 10 to dilution-1Small test tube in and shake up, be designated as 10 from dilution-1Small test tube in pipette 1 milli It is raised to dilution and is designated as 10-2Small test tube in and shake up.The rest may be inferred, pipettes dilution always and is designated as 10-6Small test tube be Only.
4th, it is coated with:
The culture medium of sterilizing is poured into flame vicinity in culture dish while hot, culture medium is covered into bottom, by used in Surface plate all to upper culture medium and be allowed to cool solidification.150 μ L are pipetted to culture dish contain strain physiology using liquid-transfering gun Saline solution.Spreading rod is cooled down on the upper lid of culture dish, on the culture dish for fill bacterium solution with spreading rod in one direction Coating, smoothens.Coated culture dish is down flat plate to be placed in constant incubator, taking-up surface plate is checked anti-after 24 hours Bacterium result.
As shown in Figure 5, after the timber of surface in situ growth nano-Ag particles is put into E. coli clones culture dish, have antibacterial Circle generates.
The present embodiment nano-Ag particles load efficiency is high, and load factor reaches 97%.

Claims (10)

  1. A kind of a kind of 1. method of wood surface growth in situ nano-Ag particles, it is characterised in that wood surface growth in situ nanometer The method of Argent grain follows the steps below:
    First, timber is immersed in Tris buffer solutions, magnetic agitation 10min~30min, then to being soaked in the Tris buffer solutions of timber Dopamine hydrochloride is added in, obtains mixture, 2h~for 24 hours is stirred at room temperature, takes out timber, the wood of taking-up then clean with deionized water Material, and under conditions of temperature is 20 DEG C~150 DEG C, 1h~48h is dried in vacuo, obtaining load has the wood of poly-dopamine coating Material;
    The Tris pH of buffer is 7.5~8.5;A concentration of 0.5mg/mL~5mg/ of Dopamine hydrochloride in the mixture mL;
    2nd, the timber that load has poly-dopamine coating is immersed in containing Ag+Solution in, at room temperature stir 30min~36h, take Go out timber, the timber taken out is then cleaned with deionized water, and under conditions of temperature is 40 DEG C~150 DEG C, be dried in vacuo 1h ~48h obtains the timber of surface in situ growth nano-Ag particles;
    Described contains Ag+Solution in Ag+A concentration of 1 × 10-3Mol/L~1mol/L.
  2. A kind of 2. method of wood surface growth in situ nano-Ag particles according to claim 1, it is characterised in that step Timber described in one is softwood or broadleaf.
  3. A kind of 3. method of wood surface growth in situ nano-Ag particles according to claim 1, it is characterised in that step Contain Ag described in two+Solution be silver nitrate solution or silver ammino solution.
  4. A kind of 4. method of wood surface growth in situ nano-Ag particles according to claim 1, it is characterised in that step The timber taken out is cleaned in one and then with deionized water, and under conditions of temperature is 60 DEG C~150 DEG C, vacuum drying 1h~ 48h。
  5. A kind of 5. method of wood surface growth in situ nano-Ag particles according to claim 1, it is characterised in that step A concentration of 1mg/mL~2mg/mL of Dopamine hydrochloride in mixture described in one.
  6. A kind of 6. method of wood surface growth in situ nano-Ag particles according to claim 1, it is characterised in that step The timber that load has poly-dopamine coating is immersed in containing Ag in two+Solution in, stir 1h~for 24 hours at room temperature.
  7. A kind of 7. method of wood surface growth in situ nano-Ag particles according to claim 1, it is characterised in that step Contain Ag described in two+Solution in Ag+A concentration of 0.5 × 10-3Mol/L~0.5 × 10-2mol/L。
  8. A kind of 8. method of wood surface growth in situ nano-Ag particles according to claim 1, it is characterised in that step Contain Ag described in two+Solution in Ag+A concentration of 5 × 10-2mol/L。
  9. A kind of 9. method of wood surface growth in situ nano-Ag particles according to claim 1, it is characterised in that step Contain Ag described in two+Solution in Ag+A concentration of 0.5mol/L.
  10. A kind of 10. method of wood surface growth in situ nano-Ag particles according to claim 1, it is characterised in that step The timber taken out is cleaned in two and then with deionized water, and under conditions of temperature is 60 DEG C~150 DEG C, vacuum drying 1h~ 48h。
CN201711405429.9A 2017-12-22 2017-12-22 A kind of method of wood surface growth in situ nano-Ag particles Pending CN108145816A (en)

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CN109623995A (en) * 2019-01-09 2019-04-16 中南林业科技大学 Photo-induced mould proof bamboo wood product and preparation method thereof
CN109732725A (en) * 2019-01-09 2019-05-10 中南林业科技大学 A kind of biological material and preparation method thereof of the load silver/titanium dioxide in situ based on poly-dopamine modification
CN109732733A (en) * 2019-01-23 2019-05-10 湖南桃花江竹材科技股份有限公司 Integratively formed bamboo sleeper and preparation method thereof
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CN109623995A (en) * 2019-01-09 2019-04-16 中南林业科技大学 Photo-induced mould proof bamboo wood product and preparation method thereof
CN109732725A (en) * 2019-01-09 2019-05-10 中南林业科技大学 A kind of biological material and preparation method thereof of the load silver/titanium dioxide in situ based on poly-dopamine modification
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CN109747008A (en) * 2019-01-23 2019-05-14 湖南桃花江竹材科技股份有限公司 A kind of bamboo sleeper of assembled formation and preparation method thereof
CN109592728A (en) * 2019-01-28 2019-04-09 东北林业大学 A kind of nano silver particles/wood composite material for water treatment and preparation method thereof
CN110154186A (en) * 2019-04-09 2019-08-23 中国林业科学研究院林业新技术研究所 A kind of aqueous wood stain and color method
CN110065109A (en) * 2019-04-26 2019-07-30 北京林业大学 A kind of wood single-plate and high-density polyethylene plastics film bonding reinforcing technology based on poly-dopamine enhancing

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