CN105922413A - Preparation method of magnetic wood material for absorbing electromagnetic wave - Google Patents
Preparation method of magnetic wood material for absorbing electromagnetic wave Download PDFInfo
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- CN105922413A CN105922413A CN201610251714.9A CN201610251714A CN105922413A CN 105922413 A CN105922413 A CN 105922413A CN 201610251714 A CN201610251714 A CN 201610251714A CN 105922413 A CN105922413 A CN 105922413A
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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
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B27—WORKING OR PRESERVING WOOD OR SIMILAR MATERIAL; NAILING OR STAPLING MACHINES IN GENERAL
- B27K—PROCESSES, APPARATUS OR SELECTION OF SUBSTANCES FOR IMPREGNATING, STAINING, DYEING, BLEACHING OF WOOD OR SIMILAR MATERIALS, OR TREATING OF WOOD OR SIMILAR MATERIALS WITH PERMEANT LIQUIDS, NOT OTHERWISE PROVIDED FOR; CHEMICAL OR PHYSICAL TREATMENT OF CORK, CANE, REED, STRAW OR SIMILAR MATERIALS
- B27K3/00—Impregnating wood, e.g. impregnation pretreatment, for example puncturing; Wood impregnation aids not directly involved in the impregnation process
- B27K3/02—Processes; Apparatus
- B27K3/08—Impregnating by pressure, e.g. vacuum impregnation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B27—WORKING OR PRESERVING WOOD OR SIMILAR MATERIAL; NAILING OR STAPLING MACHINES IN GENERAL
- B27K—PROCESSES, APPARATUS OR SELECTION OF SUBSTANCES FOR IMPREGNATING, STAINING, DYEING, BLEACHING OF WOOD OR SIMILAR MATERIALS, OR TREATING OF WOOD OR SIMILAR MATERIALS WITH PERMEANT LIQUIDS, NOT OTHERWISE PROVIDED FOR; CHEMICAL OR PHYSICAL TREATMENT OF CORK, CANE, REED, STRAW OR SIMILAR MATERIALS
- B27K3/00—Impregnating wood, e.g. impregnation pretreatment, for example puncturing; Wood impregnation aids not directly involved in the impregnation process
- B27K3/34—Organic impregnating agents
- B27K3/50—Mixtures of different organic impregnating agents
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B27—WORKING OR PRESERVING WOOD OR SIMILAR MATERIAL; NAILING OR STAPLING MACHINES IN GENERAL
- B27K—PROCESSES, APPARATUS OR SELECTION OF SUBSTANCES FOR IMPREGNATING, STAINING, DYEING, BLEACHING OF WOOD OR SIMILAR MATERIALS, OR TREATING OF WOOD OR SIMILAR MATERIALS WITH PERMEANT LIQUIDS, NOT OTHERWISE PROVIDED FOR; CHEMICAL OR PHYSICAL TREATMENT OF CORK, CANE, REED, STRAW OR SIMILAR MATERIALS
- B27K3/00—Impregnating wood, e.g. impregnation pretreatment, for example puncturing; Wood impregnation aids not directly involved in the impregnation process
- B27K3/52—Impregnating agents containing mixtures of inorganic and organic compounds
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/0018—Mixed oxides or hydroxides
- C01G49/0072—Mixed oxides or hydroxides containing manganese
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- Chemical & Material Sciences (AREA)
- Wood Science & Technology (AREA)
- Forests & Forestry (AREA)
- Inorganic Chemistry (AREA)
- Organic Chemistry (AREA)
- Nanotechnology (AREA)
- Chemical And Physical Treatments For Wood And The Like (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention discloses a preparation method of a magnetic wood material for absorbing electromagnetic wave, relates to the preparation method of the magnetic wood material and aims to solve the problem that the electromagnetic wave cannot be efficiently absorbed by using the wood material in the prior art. The method comprises the following steps: step 1, preparing a graphene sheet; step 2, preparing MnFe2O4 nanometer particles; step 3, pre-treating the wood material; step 4, gluing the surface of the wood material; step 5, preparing solid turbid liquid; step 6, dipping to finish the preparation process of the magnetic wood material for absorbing electromagnetic wave. The preparation method disclosed by the invention is used for preparing the magnetic wood material for absorbing electromagnetic wave.
Description
Technical field
The present invention relates to the preparation method of magnetic timber.
Background technology
Along with popularizing of the wireless telecommunications systems such as mobile phone, computer, router, electromagnetic radiation has been obtained for the weight of people
Depending on.In order to reduce the impact that surrounding is brought by unnecessary electromagnetic radiation, electromagnetic wave absorbent material arises at the historic moment.Timber
As building, the ornament materials of a kind of high-quality, it is widely used in all trades and professions of human lives, particularly in the family of the mankind
Occupy in life.But, as a kind of natural organic material, itself to frequency 2GHz～18GHz electromagnetic wave also
There is no Absorption.Therefore, in the information age of nowadays high speed development, develop a kind of wooden material with microwave absorption effect
Material tool is of great significance.
Summary of the invention
The invention solves the problems that prior art exist utilize timber can not the problem of efficient absorption electromagnetic wave, and provide one to be used for
The preparation method of the magnetic timber of electromagnetic wave absorption.
The preparation method of a kind of magnetic timber for electromagnetic wave absorption, specifically follows the steps below:
One, graphene film is prepared:
1., graphite powder, potassium peroxydisulfate, phosphorus pentoxide and acid solution are mixed, seal reactor, in temperature be
Hydro-thermal reaction 1h～52h at 70 DEG C～200 DEG C, be cooled to room temperature, then adds distilled water in reactor, stands 1h～24h,
Obtain mixture A；
Described graphite powder is 1:(0.1～10 with the mass ratio of potassium peroxydisulfate)；Described graphite powder and phosphorus pentoxide
Mass ratio is 1:(0.1～10)；The quality of described graphite powder and the volume ratio of acid solution are 1g:(1～1000) mL；
The quality of described graphite powder and the volume ratio of distilled water are 1g:(1～1000) mL；
Step one 1. described in acid solution be mass percent be 1%～99% sulphuric acid or mass percent be
The nitric acid of 1%～99%；
2., under conditions of temperature is 0 DEG C～30 DEG C, with speed as 0.01mL/min～10mL/min, in mixture A
Add acid solution and potassium permanganate, react 1h～52h, be subsequently adding distilled water, react 1h～52h, obtain mixture B；
Described mixture A is 1:(0.1～10 with the volume ratio of acid solution)；The volume of described mixture A and Gao Meng
The mass ratio of acid potassium is 1mL:(0.01～10) g；Described mixture A is 1:(0.1～10 with the volume ratio of distilled water)；
Step one 2. described in acid solution be mass percent be 50%～98% sulphuric acid or mass percent be
The nitric acid of 50%～98%；
3., being initially charged distilled water and hydrogen peroxide in mixture B, react 1h～52h, adding mass percent is
The hydrochloric acid solution of 1%～20% or concentration are 1.0 × 10-4The alkaline solution regulation pH of mol/L～10mol/L to neutral, then from
The heart separates, and obtains solid product, at temperature is 20 DEG C～150 DEG C, solid product is dried 1h～48h, obtains aoxidizing stone
Ink alkene；
Described mixture B is 1:(1～100 with the volume ratio of distilled water)；Described mixture B and the volume ratio of hydrogen peroxide
For 1:(0.01～10)；
4., by graphene oxide it is placed in 10s～60s in the Muffle furnace that temperature is 500 DEG C～1100 DEG C, obtains graphene film；
Two, preparation MnFe2O4Nanoparticle:
Will be containing Fe3+Salt, containing Mn2+Salt and water mixing, obtain containing Fe3+And Mn2+Mixed solution, will
Aqueous slkali adds containing Fe3+And Mn2+Mixed solution in, seal reactor, then water at temperature is 70 DEG C～200 DEG C
Thermal response 1h～52h, obtain MnFe2O4Nanoparticle；
Described containing Fe3+And Mn2+Mixed solution in containing Fe3+Salinity be 0.01mol/L～10mol/L；Described
Containing Mn2+Salt with containing Fe3+The mol ratio of salt be 1:(1～20)；Described containing Fe3+And Mn2+Mixing molten
Liquid is 1:(1～10 with the volume ratio of aqueous slkali)；
Described aqueous slkali is that concentration is the NaOH solution of 0.1mol/L～10mol/L or mass percent is 1%～10%
Ammonia spirit；
Three, the pretreatment of timber:
Graphene film step one 4. prepared mixes with distilled water, obtains graphene solution, the timber leaching that will clean up
Enter in graphene solution, and sealed reaction vessel, vacuum impregnation 1h～24h, then water at temperature is 70 DEG C～200 DEG C
Thermal response 1h～52h, then reaction vessel is cooled to room temperature, take out reacted timber, and be 20 DEG C～150 DEG C in temperature
Under conditions of, it is vacuum dried 1h～48h, obtains Graphene/Wood composite material；
The quality of described graphene film and the volume ratio of distilled water are 1g:(1～100) mL；
Four, the surface coating of timber processes:
1. Graphene/the Wood composite material, by step 3 prepared is placed in adhesive solvent I, impregnates 1min～30min,
Take out, dry in atmosphere；2., repeat step 4 1. 1 time～10 times, obtain the timber after gluing processes；
Described adhesive solvent I is carried out according to the following steps: joins in solvent orange 2 A by adhesive component A, obtains
Adhesive component A solution；Adhesive B component is joined in solvent B, obtains adhesive B component solution；By gluing
Agent component A solution mixes with adhesive B component solution, obtains adhesive solvent；Described solvent orange 2 A and solvent B are phase
Same solvent；
Described adhesive component A is epoxy resin, polrvinyl chloride or phenolic resin；Described adhesive B component is poly-
Amide, ethylenediamine, triethylene tetramine or maleic anhydride；
The quality of described adhesive component A and the volume ratio of solvent orange 2 A are 1g:(1～50) mL；Described adhesive B
The quality of component is 1g:(1～50 with the volume ratio of solvent B) mL；Described adhesive component A solution and adhesive B
The volume ratio of component solution is 1:(1～20)；
Five, solid suspension is prepared:
MnFe prepared by step 22O4Nanoparticle joins in adhesive solvent II, after being sufficiently stirred for, obtains solid
Suspension；Described adhesive solvent II is identical adhesive solvent with the adhesive solvent I described in step 4；
Described MnFe2O4The quality of nanoparticle is 1g:(1～100 with the volume ratio of adhesive solvent II) mL；
Six, impregnation process:
1. the gluing, by step 4 2. prepared process after the solid suspension prepared to step 5 of timber pickling in, dipping
1min～30min, takes out, dries 1min～30min in atmosphere；2., repeat step 6 1. 1 time～10 times, take out,
Under conditions of temperature is 45 DEG C～200 DEG C, dries 1h～52h, obtain the magnetic timber for electromagnetic wave absorption.
The invention has the beneficial effects as follows:
Prepared by the present invention can be used for the magnetic timber of electromagnetic wave absorption, and technique is simple, and raw material sources are extensive, the magnetic obtained
Timber has good magnetic and excellent electro-magnetic wave absorption performance.
The present invention is for the preparation method of a kind of magnetic timber for electromagnetic wave absorption.
Accompanying drawing explanation
Fig. 1 is the photomacrograph of the magnetic timber for electromagnetic wave absorption of embodiment one preparation；1 is embodiment one preparation
Magnetic timber for electromagnetic wave absorption；2 is Magnet；
Fig. 2 be the magnetic timber for electromagnetic wave absorption of embodiment one preparation to frequency at the electromagnetism of 2GHz～18GHz
The reflection loss figure of ripple；1 is unseasoned timber；2 is the magnetic timber for electromagnetic wave absorption of embodiment one preparation；
Fig. 3 be the Graphene/Wood composite material of contrast experiment one preparation to frequency electromagnetic wave anti-of 2GHz～18GHz
Penetrate loss figure；
Fig. 4 is the modified timber of the magnetic nano-particle of contrast experiment two preparation to frequency at the electromagnetic wave of 2GHz～18GHz
Reflection loss figure.
Detailed description of the invention
Technical solution of the present invention is not limited to the detailed description of the invention of act set forth below, also includes between each detailed description of the invention
Combination in any.
Detailed description of the invention one: the preparation method of a kind of magnetic timber for electromagnetic wave absorption described in present embodiment,
Specifically follow the steps below:
One, graphene film is prepared:
1., graphite powder, potassium peroxydisulfate, phosphorus pentoxide and acid solution are mixed, seal reactor, in temperature be
Hydro-thermal reaction 1h～52h at 70 DEG C～200 DEG C, be cooled to room temperature, then adds distilled water in reactor, stands 1h～24h,
Obtain mixture A；
Described graphite powder is 1:(0.1～10 with the mass ratio of potassium peroxydisulfate)；Described graphite powder and phosphorus pentoxide
Mass ratio is 1:(0.1～10)；The quality of described graphite powder and the volume ratio of acid solution are 1g:(1～1000) mL；
The quality of described graphite powder and the volume ratio of distilled water are 1g:(1～1000) mL；
Step one 1. described in acid solution be mass percent be 1%～99% sulphuric acid or mass percent be
The nitric acid of 1%～99%；
2., under conditions of temperature is 0 DEG C～30 DEG C, with speed as 0.01mL/min～10mL/min, in mixture A
Add acid solution and potassium permanganate, react 1h～52h, be subsequently adding distilled water, react 1h～52h, obtain mixture B；
Described mixture A is 1:(0.1～10 with the volume ratio of acid solution)；The volume of described mixture A and Gao Meng
The mass ratio of acid potassium is 1mL:(0.01～10) g；Described mixture A is 1:(0.1～10 with the volume ratio of distilled water)；
Step one 2. described in acid solution be mass percent be 50%～98% sulphuric acid or mass percent be
The nitric acid of 50%～98%；
3., being initially charged distilled water and hydrogen peroxide in mixture B, react 1h～52h, adding mass percent is
The hydrochloric acid solution of 1%～20% or concentration are 1.0 × 10-4The alkaline solution regulation pH of mol/L～10mol/L to neutral, then from
The heart separates, and obtains solid product, at temperature is 20 DEG C～150 DEG C, solid product is dried 1h～48h, obtains aoxidizing stone
Ink alkene；
Described mixture B is 1:(1～100 with the volume ratio of distilled water)；Described mixture B and the volume ratio of hydrogen peroxide
For 1:(0.01～10)；
4., by graphene oxide it is placed in 10s～60s in the Muffle furnace that temperature is 500 DEG C～1100 DEG C, obtains graphene film；
Two, preparation MnFe2O4Nanoparticle:
Will be containing Fe3+Salt, containing Mn2+Salt and water mixing, obtain containing Fe3+And Mn2+Mixed solution, will
Aqueous slkali adds containing Fe3+And Mn2+Mixed solution in, seal reactor, then water at temperature is 70 DEG C～200 DEG C
Thermal response 1h～52h, obtain MnFe2O4Nanoparticle；
Described containing Fe3+And Mn2+Mixed solution in containing Fe3+Salinity be 0.01mol/L～10mol/L；Described
Containing Mn2+Salt with containing Fe3+The mol ratio of salt be 1:(1～20)；Described containing Fe3+And Mn2+Mixing molten
Liquid is 1:(1～10 with the volume ratio of aqueous slkali)；
Described aqueous slkali is that concentration is the NaOH solution of 0.1mol/L～10mol/L or mass percent is 1%～10%
Ammonia spirit；
Three, the pretreatment of timber:
Graphene film step one 4. prepared mixes with distilled water, obtains graphene solution, the timber leaching that will clean up
Enter in graphene solution, and sealed reaction vessel, vacuum impregnation 1h～24h, then water at temperature is 70 DEG C～200 DEG C
Thermal response 1h～52h, then reaction vessel is cooled to room temperature, take out reacted timber, and be 20 DEG C～150 DEG C in temperature
Under conditions of, it is vacuum dried 1h～48h, obtains Graphene/Wood composite material；
The quality of described graphene film and the volume ratio of distilled water are 1g:(1～100) mL；
Four, the surface coating of timber processes:
1. Graphene/the Wood composite material, by step 3 prepared is placed in adhesive solvent I, impregnates 1min～30min,
Take out, dry in atmosphere；2., repeat step 4 1. 1 time～10 times, obtain the timber after gluing processes；
Described adhesive solvent I is carried out according to the following steps: joins in solvent orange 2 A by adhesive component A, obtains
Adhesive component A solution；Adhesive B component is joined in solvent B, obtains adhesive B component solution；By gluing
Agent component A solution mixes with adhesive B component solution, obtains adhesive solvent；Described solvent orange 2 A and solvent B are phase
Same solvent；
Described adhesive component A is epoxy resin, polrvinyl chloride or phenolic resin；Described adhesive B component is poly-
Amide, ethylenediamine, triethylene tetramine or maleic anhydride；
The quality of described adhesive component A and the volume ratio of solvent orange 2 A are 1g:(1～50) mL；Described adhesive B
The quality of component is 1g:(1～50 with the volume ratio of solvent B) mL；Described adhesive component A solution and adhesive B
The volume ratio of component solution is 1:(1～20)；
Five, solid suspension is prepared:
MnFe prepared by step 22O4Nanoparticle joins in adhesive solvent II, after being sufficiently stirred for, obtains solid
Suspension；Described adhesive solvent II is identical adhesive solvent with the adhesive solvent I described in step 4；
Described MnFe2O4The quality of nanoparticle is 1g:(1～100 with the volume ratio of adhesive solvent II) mL；
Six, impregnation process:
1. the gluing, by step 4 2. prepared process after the solid suspension prepared to step 5 of timber pickling in, dipping
1min～30min, takes out, dries 1min～30min in atmosphere；2., repeat step 6 1. 1 time～10 times, take out,
Under conditions of temperature is 45 DEG C～200 DEG C, dries 1h～52h, obtain the magnetic timber for electromagnetic wave absorption.
Present embodiment provides the benefit that:
Prepared by present embodiment can be used for the magnetic timber of electromagnetic wave absorption, and technique is simple, and raw material sources are extensive, obtain
Magnetic timber has good magnetic and excellent electro-magnetic wave absorption performance.
Detailed description of the invention two: present embodiment is unlike detailed description of the invention one: step one 3. described in alkalescence
Solution is NaOH solution, KOH solution or ammonia spirit.Other is identical with detailed description of the invention one.
Detailed description of the invention three: present embodiment is unlike one of detailed description of the invention one or two: in step 2
Described containing Fe3+Salt be iron chloride, iron sulfate or ferric nitrate.Other is identical with detailed description of the invention one or two.
Detailed description of the invention four: present embodiment is unlike one of detailed description of the invention one to three: in step 2
Described containing Mn2+Salt be manganese chloride, manganese sulfate or manganese nitrate.Other is identical with detailed description of the invention one to three.
Detailed description of the invention five: present embodiment is unlike one of detailed description of the invention one to four: in step 3
Described timber is softwood or broadleaf.Other is identical with detailed description of the invention one to four.
Detailed description of the invention six: present embodiment is unlike one of detailed description of the invention one to five: in step 4
Described solvent orange 2 A is ethyl acetate, acetone or oxolane.Other is identical with detailed description of the invention one to five.
Detailed description of the invention seven: present embodiment is unlike one of detailed description of the invention one to six: in step 4
Described solvent B is ethyl acetate, acetone or oxolane.Other is identical with detailed description of the invention one to six.
Detailed description of the invention eight: present embodiment is unlike one of detailed description of the invention one to seven: in step 2
Described containing Fe3+And Mn2+Mixed solution in containing Fe3+Salinity be 0.02mol/L；Described containing Mn2+
Salt with containing Fe3+The mol ratio of salt be 1:2；Described containing Fe3+And Mn2+The volume of mixed solution and aqueous slkali
Ratio is 1:1.Other is identical with detailed description of the invention one to seven.
Detailed description of the invention nine: present embodiment is unlike one of detailed description of the invention one to eight: in step 3
Graphene film step one 4. prepared mixes with distilled water, obtains graphene solution, is immersed in by the timber cleaned up
In graphene solution, and sealed reaction vessel, vacuum impregnation 6h, then hydro-thermal reaction 12h at temperature is 100 DEG C, then
Reaction vessel is cooled to room temperature, takes out reacted timber, and under conditions of temperature is 103 DEG C, be vacuum dried 24h,
Obtain Graphene/Wood composite material.Other is identical with detailed description of the invention one to eight.
Detailed description of the invention ten: present embodiment is unlike one of detailed description of the invention one to nine: in step 5
Described MnFe2O4The quality of nanoparticle is 1g:1mL with the volume ratio of adhesive solvent II.Other be embodied as
Mode one to nine is identical.
Employing following example checking beneficial effects of the present invention:
Embodiment one:
A kind of preparation method for the magnetic timber of electromagnetic wave absorption is to sequentially include the following steps:
One, graphene film is prepared:
1., graphite powder, potassium peroxydisulfate, phosphorus pentoxide and acid solution are mixed, seal reactor, in temperature be
Hydro-thermal reaction 6h at 80 DEG C, is cooled to room temperature, then adds distilled water in reactor, stands 12h, obtain mixture A；
Described graphite powder is 1:1 with the mass ratio of potassium peroxydisulfate；Described graphite powder and the mass ratio of phosphorus pentoxide
For 1:1；The quality of described graphite powder and the volume ratio of acid solution are 1g:5mL；The quality of described graphite powder
It is 1g:100mL with the volume ratio of distilled water；
Step one 1. described in acid solution be mass percent be the sulphuric acid of 98%；
2., under conditions of temperature is 0 DEG C, with speed as 0.1mL/min, in mixture A, acid solution and height are added
Potassium manganate, reacts 4h, is subsequently adding distilled water, reacts 4h, obtains mixture B；
Described mixture A is 1:0.2 with the volume ratio of acid solution；The volume of described mixture A and potassium permanganate
Mass ratio is 1mL:0.03g；Described mixture A is 1:0.5 with the volume ratio of distilled water；
Step one 2. described in acid solution be mass percent be the sulphuric acid of 98%；
3., being initially charged distilled water and hydrogen peroxide in mixture B, react 4h, adding mass percent is 25%
Hydrochloric acid solution or the alkaline solution regulation pH that concentration is 0.1mol/L are the most neutral, are then centrifuged for separating, obtain solid product,
At temperature is 100 DEG C, solid product is dried 12h, obtains graphene oxide；
Step one 3. described in aqueous slkali be KOH solution；
Described mixture B is 1:1 with the volume ratio of distilled water；Described mixture B with the volume ratio of hydrogen peroxide is
1:0.01；
4., by graphene oxide it is placed in 30s in the Muffle furnace that temperature is 1050 DEG C, obtains graphene film；
Two, preparation MnFe2O4Nanoparticle:
Will be containing Fe3+Salt, containing Mn2+Salt and water mixing, obtain containing Fe3+And Mn2+Mixed solution, will
Aqueous slkali adds containing Fe3+And Mn2+Mixed solution in, seal reactor, then at temperature is 120 DEG C, hydro-thermal is anti-
Answer 12h, obtain MnFe2O4Nanoparticle；
Described containing Fe3+And Mn2+Mixed solution in containing Fe3+Salinity be 0.02mol/L；Described contains
Mn2+Salt with containing Fe3+The mol ratio of salt be 1:2；Described containing Fe3+And Mn2+Mixed solution and aqueous slkali
Volume ratio be 1:1；
Described aqueous slkali be concentration be the NaOH solution of 1mol/L；
Described containing Fe3+Salt be iron chloride；Described containing Mn2+Salt be manganese chloride；
Three, the pretreatment of timber:
Graphene film step one 4. prepared mixes with distilled water, obtains graphene solution, the timber leaching that will clean up
Enter in graphene solution, and sealed reaction vessel, vacuum impregnation 6h, then hydro-thermal reaction 12h at temperature is 100 DEG C,
Again reaction vessel is cooled to room temperature, takes out reacted timber, and under conditions of temperature is 103 DEG C, be vacuum dried 24h,
Obtain Graphene/Wood composite material；
The quality of described graphene film and the volume ratio of distilled water are 1g:100mL；
Described timber is broadleaf；
Four, the surface coating of timber processes:
1. Graphene/the Wood composite material, by step 3 prepared is placed in adhesive solvent I, impregnates 10min, takes out,
Dry in atmosphere；2., repeat step 4 1. 10 times, obtain the timber after gluing processes；
Described adhesive solvent I is carried out according to the following steps: joins in solvent orange 2 A by adhesive component A, obtains
Adhesive component A solution；Adhesive B component is joined in solvent B, obtains adhesive B component solution；By gluing
Agent component A solution mixes with adhesive B component solution, obtains adhesive solvent；Described solvent orange 2 A and solvent B are phase
Same solvent；
Described adhesive component A is epoxy resin；Adhesive B component described in step is polyamide；
The quality of described adhesive component A and the volume ratio of solvent orange 2 A are 1g:1mL；Described adhesive B component
The volume ratio of quality and solvent B be 1g:2mL；Described adhesive component A solution and adhesive B component solution
Volume ratio be 1:1；
Described solvent orange 2 A is ethyl acetate；Described solvent B is ethyl acetate；
Five, solid suspension is prepared:
MnFe prepared by step 22O4Nanoparticle joins in adhesive solvent II, after being sufficiently stirred for, obtains solid
Suspension；Described adhesive solvent II is identical adhesive solvent with the adhesive solvent I described in step 4；
Described MnFe2O4The quality of nanoparticle is 1g:1mL with the volume ratio of adhesive solvent II；
Six, impregnation process:
1. the gluing, by step 4 2. prepared process after the solid suspension prepared to step 5 of timber pickling in, dipping
10min, takes out, dries 30min in atmosphere；2., repeat step 6 1. 5 times, take out, at the bar that temperature is 60 DEG C
Under part, dry 24h, obtain the magnetic timber for electromagnetic wave absorption.
Fig. 1 is the photomacrograph of the magnetic timber for electromagnetic wave absorption of embodiment one preparation；1 is embodiment one preparation
Magnetic timber for electromagnetic wave absorption；2 is Magnet, as seen from the figure, and wood surface energy strong bond magnetic nano-particle,
And make timber be provided with good magnetic.
Fig. 2 be the magnetic timber for electromagnetic wave absorption of embodiment one preparation to frequency at the electromagnetism of 2GHz～18GHz
The reflection loss figure of ripple；1 is unseasoned timber；2 is the magnetic timber for electromagnetic wave absorption of embodiment one preparation；By
Figure understands, and for the magnetic timber of electromagnetic wave absorption under the Electromagnetic Field that frequency is 8GHz, its reflection loss can reach
To 18dB, and in the range of frequency 6.5～8.2GHz, its reflection loss can reach more than-10dB, illustrates at this frequency
In the range of rate, the timber after this process can absorb the electromagnetic wave of more than 90%, can serve as a kind of effective suction ripple material
Material.
Contrast experiment one:
One, graphene film is prepared:
1., graphite powder, potassium peroxydisulfate, phosphorus pentoxide and acid solution are mixed, seal reactor, in temperature be
Hydro-thermal reaction 6h at 80 DEG C, is cooled to room temperature, then adds distilled water in reactor, stands 12h, obtain mixture A；
Described graphite powder is 1:1 with the mass ratio of potassium peroxydisulfate；Described graphite powder and the mass ratio of phosphorus pentoxide
For 1:1；The quality of described graphite powder and the volume ratio of acid solution are 1g:5mL；The quality of described graphite powder
It is 1g:100mL with the volume ratio of distilled water；
Step one 1. described in acid solution be mass percent be the sulphuric acid of 98%；
2., under conditions of temperature is 0 DEG C, with speed as 0.1mL/min, in mixture A, acid solution and height are added
Potassium manganate, reacts 4h, is subsequently adding distilled water, reacts 4h, obtains mixture B；
Described mixture A is 1:0.2 with the volume ratio of acid solution；The volume of described mixture A and potassium permanganate
Mass ratio is 1mL:0.03g；Described mixture A is 1:0.5 with the volume ratio of distilled water；
Step one 2. described in acid solution be mass percent be the sulphuric acid of 98%；
3., being initially charged distilled water and hydrogen peroxide in mixture B, react 4h, adding mass percent is 25%
Hydrochloric acid solution or the alkaline solution regulation pH that concentration is 0.1mol/L are the most neutral, are then centrifuged for separating, obtain solid product,
At temperature is 100 DEG C, solid product is dried 12h, obtains graphene oxide；
Step one 3. described in aqueous slkali be KOH solution；
Described mixture B is 1:1 with the volume ratio of distilled water；Described mixture B with the volume ratio of hydrogen peroxide is
1:0.01；
4., by graphene oxide it is placed in 30s in the Muffle furnace that temperature is 1050 DEG C, obtains graphene film；
Two, Graphene/Wood composite material is prepared:
Graphene film step one 4. prepared mixes with distilled water, obtains graphene solution, the timber leaching that will clean up
Enter in graphene solution, and sealed reaction vessel, vacuum impregnation 6h, then hydro-thermal reaction 12h at temperature is 100 DEG C,
Again reaction vessel is cooled to room temperature, takes out reacted timber, and under conditions of temperature is 103 DEG C, be vacuum dried 24h,
Obtain Graphene/Wood composite material；
The quality of described graphene film and the volume ratio of distilled water are 1g:100mL；
Described timber is broadleaf.
Fig. 3 be the Graphene/Wood composite material of contrast experiment one preparation to frequency electromagnetic wave anti-of 2GHz～18GHz
Penetrate loss figure；The timber reflection of maximum under the electromagnetic wave that frequency is 16GHz the most only processed with Graphene is damaged
Consume only 4dB, illustrate that its absorbing property is unsatisfactory.
Contrast experiment two:
One, preparation MnFe2O4Nanoparticle:
Will be containing Fe3+Salt, containing Mn2+Salt and water mixing, obtain containing Fe3+And Mn2+Mixed solution, will
Aqueous slkali adds containing Fe3+And Mn2+Mixed solution in, seal reactor, then at temperature is 120 DEG C, hydro-thermal is anti-
Answer 12h, obtain MnFe2O4Nanoparticle；
Described containing Fe3+And Mn2+Mixed solution in containing Fe3+Salinity be 0.02mol/L；Described contains
Mn2+Salt with containing Fe3+The mol ratio of salt be 1:2；Described containing Fe3+And Mn2+Mixed solution and aqueous slkali
Volume ratio be 1:1；
Described aqueous slkali be concentration be the NaOH solution of 1mol/L；
Described containing Fe3+Salt be iron chloride；Described containing Mn2+Salt be manganese chloride；
Two, the surface coating of timber processes:
1., the timber cleaned up is placed in adhesive solvent I, impregnates 10min, take out, dry in atmosphere；②、
Repeat step 2 1. 10 times, obtain the timber after gluing processes；Described timber is broadleaf；
Described adhesive solvent I is carried out according to the following steps: joins in solvent orange 2 A by adhesive component A, obtains
Adhesive component A solution；Adhesive B component is joined in solvent B, obtains adhesive B component solution；By gluing
Agent component A solution mixes with adhesive B component solution, obtains adhesive solvent；Described solvent orange 2 A and solvent B are phase
Same solvent；
Described adhesive component A is epoxy resin；Adhesive B component described in step is polyamide；
The quality of described adhesive component A and the volume ratio of solvent orange 2 A are 1g:1mL；Described adhesive B component
The volume ratio of quality and solvent B be 1g:2mL；Described adhesive component A solution and adhesive B component solution
Volume ratio be 1:1；
Described solvent orange 2 A is ethyl acetate；Described solvent B is ethyl acetate；
Three, solid suspension is prepared:
MnFe prepared by step one2O4Nanoparticle joins in adhesive solvent II, after being sufficiently stirred for, obtains solid
Suspension；Described adhesive solvent II is identical adhesive solvent with the adhesive solvent I described in step 4；
Described MnFe2O4The quality of nanoparticle is 1g:1mL with the volume ratio of adhesive solvent II；
Four, impregnation process:
1. the gluing, by step 2 2. prepared process after the solid suspension prepared to step 3 of timber pickling in, dipping
10min, takes out, dries 30min in atmosphere；2., repeat step 4 1. 5 times, take out, at the bar that temperature is 60 DEG C
Under part, dry 24h, obtain the timber that magnetic nano-particle is modified.
Fig. 4 is the modified timber of the magnetic nano-particle of contrast experiment two preparation to frequency at the electromagnetic wave of 2GHz～18GHz
Reflection loss figure；Use MnFe as seen from the figure2O4The reflection loss that the timber of coating is maximum under the electromagnetic wave of 16GHz
Having reached 5dB, the timber after processing than Graphene is slightly higher, but its wave-absorbing effect is the most undesirable.
The effect data of embodiment one be greater than contrast experiment one and contrast experiment two data add and, by gluing
MnFe2O4Nanoparticle, due to magnetic and the structure effect of nanoparticle of its excellence, can improve between timber and air
Impedance matching, thus reduce electromagnetic wave reflection in timber interface, make more electromagnetic wave enter timber.Work as electricity
Magnetic wave enters material internal, MnFe2O4Nanoparticle also will occur polarization, produce magnetic domain resonance and eddy current loss, can
With the generation assimilation effect to electromagnetic wave.Meanwhile, by preprocessing process, firm with hydrogen bond formation between Graphene and timber
In conjunction with, thus improve generation polarization between the dielectric properties of timber, beneficially electronics, when more electromagnetic wave enters
During wood internal, the dielectric loss effect strengthened in electromagnetic field due to timber, cause the absorption efficiency to electromagnetic wave to increase.
On the other hand, when more electromagnetic wave enters wood internal, due to porous and the architectural feature of anisotropic of timber,
Contributing to electromagnetic wave and produce multiple scattering, the scattering process of this reinforcement is also beneficial to increase the probability of electromagnetic wave loss.Pass through
Impedance matching, magnetic loss, dielectric loss, and multiple scattering effect serves such technique effect jointly.
Claims (10)
1. the preparation method of magnetic timber for electromagnetic wave absorption, it is characterised in that a kind of for electromagnetic wave absorption
The preparation method of magnetic timber follows the steps below:
One, graphene film is prepared:
1., graphite powder, potassium peroxydisulfate, phosphorus pentoxide and acid solution are mixed, seal reactor, in temperature be
Hydro-thermal reaction 1h～52h at 70 DEG C～200 DEG C, be cooled to room temperature, then adds distilled water in reactor, stands 1h～24h,
Obtain mixture A；
Described graphite powder is 1:(0.1～10 with the mass ratio of potassium peroxydisulfate)；Described graphite powder and phosphorus pentoxide
Mass ratio is 1:(0.1～10)；The quality of described graphite powder and the volume ratio of acid solution are 1g:(1～1000) mL；Institute
The quality of the graphite powder stated and the volume ratio of distilled water are 1g:(1～1000) mL；
Step one 1. described in acid solution be mass percent be 1%～99% sulphuric acid or mass percent be 1%～99%
Nitric acid；
2., under conditions of temperature is 0 DEG C～30 DEG C, with speed as 0.01mL/min～10mL/min, add in mixture A
Enter acid solution and potassium permanganate, react 1h～52h, be subsequently adding distilled water, react 1h～52h, obtain mixture B；
Described mixture A is 1:(0.1～10 with the volume ratio of acid solution)；The volume of described mixture A and permanganic acid
The mass ratio of potassium is 1mL:(0.01～10) g；Described mixture A is 1:(0.1～10 with the volume ratio of distilled water)；
Step one 2. described in acid solution be mass percent be 50%～98% sulphuric acid or mass percent be
The nitric acid of 50%～98%；
3., being initially charged distilled water and hydrogen peroxide in mixture B, react 1h～52h, adding mass percent is 1%～20%
Hydrochloric acid solution or concentration be 1.0 × 10-4The alkaline solution regulation pH of mol/L～10mol/L, to neutral, is then centrifuged for separating,
Obtain solid product, at temperature is 20 DEG C～150 DEG C, solid product is dried 1h～48h, obtains graphene oxide；
Described mixture B is 1:(1～100 with the volume ratio of distilled water)；Described mixture B and the volume ratio of hydrogen peroxide
For 1:(0.01～10)；
4., by graphene oxide it is placed in 10s～60s in the Muffle furnace that temperature is 500 DEG C～1100 DEG C, obtains graphene film；
Two, preparation MnFe2O4Nanoparticle:
Will be containing Fe3+Salt, containing Mn2+Salt and water mixing, obtain containing Fe3+And Mn2+Mixed solution, by alkali
Solution adds containing Fe3+And Mn2+Mixed solution in, seal reactor, then at temperature is 70 DEG C～200 DEG C, hydro-thermal is anti-
Answer 1h～52h, obtain MnFe2O4Nanoparticle；
Described containing Fe3+And Mn2+Mixed solution in containing Fe3+Salinity be 0.01mol/L～10mol/L；Described
Containing Mn2+Salt with containing Fe3+The mol ratio of salt be 1:(1～20)；Described containing Fe3+And Mn2+Mixed solution
It is 1:(1～10 with the volume ratio of aqueous slkali)；
Described aqueous slkali be concentration be the NaOH solution of 0.1mol/L～10mol/L or ammonia that mass percent is 1%～10%
Aqueous solution；
Three, the pretreatment of timber:
Graphene film step one 4. prepared mixes with distilled water, obtains graphene solution, the timber leaching that will clean up
Enter in graphene solution, and sealed reaction vessel, vacuum impregnation 1h～24h, then hydro-thermal at temperature is 70 DEG C～200 DEG C
Reaction 1h～52h, then reaction vessel is cooled to room temperature, take out reacted timber, and be 20 DEG C～the bar of 150 DEG C in temperature
Under part, it is vacuum dried 1h～48h, obtains Graphene/Wood composite material；
The quality of described graphene film and the volume ratio of distilled water are 1g:(1～100) mL；
Four, the surface coating of timber processes:
1. Graphene/the Wood composite material, by step 3 prepared is placed in adhesive solvent I, impregnates 1min～30min, takes
Go out, dry in atmosphere；2., repeat step 4 1. 1 time～10 times, obtain the timber after gluing processes；
Described adhesive solvent I is carried out according to the following steps: joins in solvent orange 2 A by adhesive component A, obtains
Adhesive component A solution；Adhesive B component is joined in solvent B, obtains adhesive B component solution；By gluing
Agent component A solution mixes with adhesive B component solution, obtains adhesive solvent；Described solvent orange 2 A and solvent B are phase
Same solvent；
Described adhesive component A is epoxy resin, polrvinyl chloride or phenolic resin；Described adhesive B component is polyamides
Amine, ethylenediamine, triethylene tetramine or maleic anhydride；
The quality of described adhesive component A and the volume ratio of solvent orange 2 A are 1g:(1～50) mL；Described adhesive B
The quality of component is 1g:(1～50 with the volume ratio of solvent B) mL；Described adhesive component A solution and adhesive B group
The volume ratio dividing solution is 1:(1～20)；
Five, solid suspension is prepared:
MnFe prepared by step 22O4Nanoparticle joins in adhesive solvent II, after being sufficiently stirred for, obtains solid
Suspension；Described adhesive solvent II is identical adhesive solvent with the adhesive solvent I described in step 4；
Described MnFe2O4The quality of nanoparticle is 1g:(1～100 with the volume ratio of adhesive solvent II) mL；
Six, impregnation process:
1. the gluing, by step 4 2. prepared process after the solid suspension prepared to step 5 of timber pickling in, dipping
1min～30min, takes out, dries 1min～30min in atmosphere；2., repeat step 6 1. 1 time～10 times, take out,
Under conditions of temperature is 45 DEG C～200 DEG C, dries 1h～52h, obtain the magnetic timber for electromagnetic wave absorption.
The preparation method of a kind of magnetic timber for electromagnetic wave absorption the most according to claim 1, its feature exists
In step one 3. described in alkaline solution be NaOH solution, KOH solution or ammonia spirit.
The preparation method of a kind of magnetic timber for electromagnetic wave absorption the most according to claim 1, its feature exists
In described in step 2 containing Fe3+Salt be iron chloride, iron sulfate or ferric nitrate.
The preparation method of a kind of magnetic timber for electromagnetic wave absorption the most according to claim 1, its feature exists
In described in step 2 containing Mn2+Salt be manganese chloride, manganese sulfate or manganese nitrate.
The preparation method of a kind of magnetic timber for electromagnetic wave absorption the most according to claim 1, its feature exists
It is softwood or broadleaf in the timber described in step 3.
The preparation method of a kind of magnetic timber for electromagnetic wave absorption the most according to claim 1, its feature exists
It is ethyl acetate, acetone or oxolane in the solvent orange 2 A described in step 4.
The preparation method of a kind of magnetic timber for electromagnetic wave absorption the most according to claim 1, its feature exists
It is ethyl acetate, acetone or oxolane in the solvent B described in step 4.
The preparation method of a kind of magnetic timber for electromagnetic wave absorption the most according to claim 1, its feature exists
In described in step 2 containing Fe3+And Mn2+Mixed solution in containing Fe3+Salinity be 0.02mol/L；Described
Containing Mn2+Salt with containing Fe3+The mol ratio of salt be 1:2；Described containing Fe3+And Mn2+Mixed solution molten with alkali
The volume ratio of liquid is 1:1.
The preparation method of a kind of magnetic timber for electromagnetic wave absorption the most according to claim 1, its feature exists
In step 3, the graphene film that 4. step one is prepared is mixed with distilled water, obtain graphene solution, by clean up
Timber is immersed in graphene solution, and sealed reaction vessel, vacuum impregnation 6h, and then at temperature is 100 DEG C, hydro-thermal is anti-
Answer 12h, then reaction vessel is cooled to room temperature, take out reacted timber, and under conditions of temperature is 103 DEG C, vacuum
It is dried 24h, obtains Graphene/Wood composite material.
The preparation method of a kind of magnetic timber for electromagnetic wave absorption the most according to claim 1, its feature exists
In the MnFe described in step 52O4The quality of nanoparticle is 1g:1mL with the volume ratio of adhesive solvent II.
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| CN106827134A (en) * | 2017-02-10 | 2017-06-13 | 南京林业大学 | A kind of preparation method of the controllable magnetic timber of magnetic |
| CN106827139A (en) * | 2017-01-18 | 2017-06-13 | 浙江省林业科学研究院 | The hydrophobic bamboo wood and its production technology of a kind of area load graphene oxide and silica |
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| CN107283566A (en) * | 2017-04-24 | 2017-10-24 | 中国林业科学研究院木材工业研究所 | Musical instrument fingerboard wood materials and preparation method thereof and its acoustic function body maceration extract |
| CN113340153A (en) * | 2021-05-20 | 2021-09-03 | 西北工业大学 | Infrared-radar compatible stealth material based on raw wood and preparation method |
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| CN113340153A (en) * | 2021-05-20 | 2021-09-03 | 西北工业大学 | Infrared-radar compatible stealth material based on raw wood and preparation method |
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