CN105885231B - A kind of composite material with electromagenetic wave radiation safeguard function and preparation method thereof - Google Patents
A kind of composite material with electromagenetic wave radiation safeguard function and preparation method thereof Download PDFInfo
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Abstract
The present invention discloses a kind of composite material with electromagenetic wave radiation safeguard function and preparation method thereof.The composite material is by 0.9 1.3 parts of dielectric loss type nanocomposite A, 1.5 2 parts of load BaFe12O19The raw materials such as halloysite nanotubes, 0.4 0.6 parts of methacryloxypropyl trimethoxy silanes, 0.8 1.2 parts of dielectric loss type nanocomposite B, 0.5 0.8 parts of γ (2,3 glycidoxy) propyl trimethoxy silicanes, 22 32 parts of polypropylene be made.Gained composite material has strong microwave attenuation characteristics, can be applied to the electromagnetic wave proof of all kinds of key buildings.
Description
Technical field
The invention belongs to field of compound material, and in particular to a kind of composite material with electromagenetic wave radiation safeguard function and
Its preparation method.
Background technology
Current from the electromagnet radiation getting worse for the transmitting station etc. that communicates in microwave base station and high-power wireless.It adopts
It can be with the electromagnetic wave of effective attenuation Discussion on architecture with the construction material with electromagnetic wave absorption function.Such as patent ZL
201010266982.0 prepare a kind of lightweight high tenacity wave absorption concretes, 8 ~ 18 GHz frequency range internal reflections rates be less than-
The bandwidth of 7dB is 10GHz.Preferable electromagenetic wave radiation protective materials need to possess that electromagnetic parameter is adjustable, electromagnetic consumable is big and proportion
Light characteristic.Homogenous material can not meet electromagenetic wave radiation requirement of shelter.There is one kind of the present invention electromagenetic wave radiation to protect work(
Can composite material, the nano-particle with different special electromagnetic performances is combined, including can effectively improving concrete etc.
A variety of building materials to the drain performance of electromagnetic wave.
The content of the invention
It is an object of the invention to provide a kind of composite materials with electromagenetic wave radiation safeguard function and preparation method thereof.
Gained composite material has strong microwave attenuation characteristics, can be applied to the electromagnetic wave proof of all kinds of key buildings.
To achieve the above object, the present invention adopts the following technical scheme that：
A kind of composite material with electromagenetic wave radiation safeguard function is made by following raw material：0.9-1.3 parts of Jie
A, 1.5-2 parts of load BaFe of dielectric loss type nanocomposite12O19Halloysite nanotubes, 0.4-0.6 parts of methacryloxypropyls
B, 0.5-0.8 parts of γ of base propyl trimethoxy silicane, 0.8-1.2 parts of dielectric loss type nanocomposites-(the third oxygen of 2,3- epoxies
Base) propyl trimethoxy silicane, 22-32 parts of polypropylene.
The preparation process of the composite material is as follows：
（1）BaFe will be loaded12O19Halloysite nanotubes and methacryloxypropyl trimethoxy silane in room temperature
After 3 h of lower stirring, 12 parts of polypropylene are added in, stir the mixture of formation nanocomposite containing magnetic loss type after 3 h, for use；
（2）At room temperature, dielectric loss type nanocomposite A is taken, 0.3-0.6 parts of γ-(2,3- the third oxygen of epoxy are added dropwise
Base) propyl trimethoxy silicane, after stirring 1 h, add in 10-20 parts of polypropylene and stir 1.5 h；Dielectric loss type is added to receive
0.2 part of γ-(2,3- glycidoxy) propyl trimethoxy silicane is added dropwise in nano composite material B, after stirring 1 h, with step (1)
The mixture of gained is fitted into high-speed mixer simultaneously, and 2-3 h are disperseed under 300-350 r/min rotating speeds；It then heats to
It 110-115 DEG C, after handling 20-25 min under 450-550 r/min rotating speeds, is transferred in cold mixing pot, treats that temperature is down to 50-55 DEG C
When blowing obtain just batch mixing；
（3）By just batch mixing is placed in the twin-screw that temperature is 170-180 DEG C, rotating speed is 70-80 r/min obtained by step (2)
It is squeezed out after being kneaded 1-1.5 h in extruder, obtains mixing materials；
（4）By mixing materials pulverization process obtained by step (3) to get to the composite wood with electromagenetic wave radiation safeguard function
Material.
Wherein load BaFe12O19Halloysite nanotubes prepare it is as follows：
（1）At 20-22 DEG C, 20.41 parts of ferric nitrate (III) nonahydrates and 1.1 parts of barium nitrates are added to 150 parts
It is for use after 2 h of stirring in ionized water；
（2）At 28-30 DEG C and under stirring, by 15.1 parts of 2- hydroxy propanes -1,2,3- tricarboxylic acids is added dropwise to the water of step (1)
In solution, time for adding is 0.5 h；Continue to be placed at room temperature for for use after stirring 3 h after being added dropwise；
（3）The ammonium hydroxide that 6.1 parts of concentration are 20 % is added dropwise in the solution of step (2), time for adding is 1 h；
（4）The halloysite nanotubes of 3.3 parts of activated processing are added in the solution of step (3), it is acute after 2 h of ultrasound
1 h of strong stirring then heats to 87-88 DEG C, and room temperature is for use after stirring 5.5 h.
（5）After the mixture of step (4) is handled 4.5 h at 123-125 DEG C, continue to handle 4 at 855-857 DEG C
H obtains load BaFe12O19Halloysite nanotubes.
The preparation process of the halloysite nanotubes of wherein activated processing is as follows：
（1）Halloysite nanotubes are taken, it is for use after mechanical crushing is handled and 350 mesh sieves is used to select；
（2）Respectively be packed into two 6 identical L nylon tanks 50 a diameter of 5 mm stainless steel ball and 40 it is a diameter of
The stainless steel ball of 10 mm, is then respectively adding step（1）2.6 kg of halloysite nanotubes, then that 360 ml are added dropwise respectively is anhydrous
Ethyl alcohol, and sealed with nylon lid.Two ball grinders are symmetrically put into planetary ball mill, are 350 rpm and every in rotating speed
Under conditions of 30 minutes automatic conversion direction of rotation after 50 h of ball milling, the chopped galapectite nanometer that length is 210-240 nm is obtained
Pipe；
（3）By step（2）The gained halloysite nanotubes that are chopped are added to 20 water of Tween that pH is 8, concentration is 15 wt%
24 h of ultrasound in solution, filtering, after being eluted with water, are dried in vacuo after 30 h to get the Ai Luo of activated processing at 68-70 DEG C
Stone nanotube.
The preparation process of its dielectric loss type nanocomposite A is as follows：
（1）Under room temperature and stirring condition, 0.5 part of alkylphenol polyoxyethylene ether and 0.65 part of ammonium sulfate are added to 22 parts
It is for use after 3 h of stirring in ionized water；
（2）The modification halloysite nanotubes of 1.6 parts of load Nanometer Coppers are added in, after stirring 2 h, then 1 h of ultrasound, it is cooled to 1-
3 DEG C for use；
（3）0.85 part of titanium tetrachloride is added, is vigorously stirred 3 h；23-25 DEG C is then heated to, continues to be vigorously stirred 1.5
After h, ammonium hydroxide is added dropwise, time for adding is 1 h；Continue to stir 0.5 h after being added dropwise, filter, after powder is cleaned with pure water,
24 h are dried in vacuo at 65 DEG C, obtain dielectric loss type nanocomposite A, the wherein average grain diameter of Nanometer Copper crystal grain is 2-6
nm。
The preparation process of its dielectric loss type nanocomposite B is as follows：
（1）Under the gentle agitation of room, 5.4 parts of sodium chloride are added in 28 parts of deionized waters, continue to stir for use after 1 h；
（2）The halloysite nanotubes that 1.95 parts of surfaces are modified are added in the aqueous solution of step (1), are vigorously stirred 2 h
Afterwards, then 1 h of ultrasound, 6.2 parts of dimethyl diallyl ammonium chloride-acrylamide copolymers are then added in, are vigorously stirred mistake after 2 h
Filter, it is for use after powder is cleaned with pure water；
（3）Under the gentle agitation of room, 5.85 parts of kayexalates are added in 16 parts of deionized waters, continue to stir
After 2 h, the powder that step (2) is got ready is added in, filters, powder is cleaned with pure water, for use after being vigorously stirred 2.5 h；
（4）The powder of step (3) is added in 17 parts of deionized waters, after stirring 2 h, adds in 6.2 parts of dimethyl diene
Propyl ammonium chloride-acrylamide copolymer filters after being vigorously stirred 3 h, for use after powder is cleaned with pure water；
（5）Under the gentle agitation of room, the powder of step (4) and 3.0 parts of octyl phenol polyoxyethylene ether are added to 22 simultaneously
In part deionized water, continue after stirring 2 h, add in 103 parts of 2- hydroxy propanes -1,2,3- tricarboxylic acids simultaneously stirs 0.5 h, Ran Houjia
Enter 1.5 part of six hydration Nickel Chloride, be vigorously stirred 3 h, then be cooled to 1-3 DEG C, obtain solution for later use；
（6）At 1-3 DEG C, 5.8 parts of sodium borohydrides are added in 20 parts of ionized waters, after stirring 15 min, at 1-3 DEG C and
It is vigorously stirred down, is added drop-wise in the solution of step (5), time for adding is 1 h；It is filtered after being added dropwise, powder is washed with pure water
After net, 30 h are dried in vacuo at 70 DEG C, obtain dielectric loss type nanocomposite B.Wherein nanometer titanium dioxide nickel particle
Average grain diameter is 3-6 nm.
Wherein surface is modified halloysite nanotubes and comprises the following steps：
By 3.2 kg of halloysite nanotubes of activated processing, it is added in 46 L chloroforms, under nitrogen protection room
After temperature is ultrasonically treated 5 h, adds in 122 ml boron trifluoride etherates and 4.5 h are stirred at room temperature；It -10 ~ 12 DEG C and is stirring again
Under the conditions of mixing, 610 ml 3- methyl -3- oxetane methanols are slowly added dropwise in the 8 h times of control, are added dropwise after -9 ~ 11
DEG C continue to stir 24 h；Then 900 ml absolute ethyl alcohols are added in, by 0.5 h of rotating speed centrifugal treating of 5000-5300 rpm, separation
Recycling design, powder are cleaned through absolute ethyl alcohol, and are dried in vacuo 20 h at room temperature, obtain the modification of 3.47-3.61 kg surfaces
Halloysite nanotubes.
The modification halloysite nanotubes for wherein loading Nanometer Copper comprise the following steps：
（1）Under the gentle agitation of room, 7.15 parts of potassium chloride are added in 50 parts of deionized waters, continue to treat after stirring 1.5 h
With；
（2）It adds in 2.89 parts of surfaces and is modified halloysite nanotubes, after stirring 2 h, then 2 h of ultrasound, then add in 7.53 parts
Diallyl dimethyl ammoniumchloride filters after being vigorously stirred 6 h, for use after powder is cleaned with pure water；
（3）Under the gentle agitation of room, 9.4 parts of poly- naphthalene formaldehyde sulfonates are added in 25 parts of deionized waters, stir 5 h
Afterwards, add in the powder that step (2) is got ready, filtered after being vigorously stirred 5 h, by powder pure water cleaned standby seam；
（4）Under the gentle agitation of room, by 1.2 parts of 2- hydroxysuccinic acids and 6.25 parts of alkylphenol polyoxyethylene ether and step
(3) powder got ready is added in deionized water simultaneously, is continued after stirring 1.5 h, is added in 1.62 parts of Copper dichloride dihydrates, acute
4 h of ultrasound after 1 h of strong stirring, obtain solution for later use；
（5）At 1-3 DEG C, 7.35 parts of sodium borohydrides are added in 28 parts of deionized waters, after stirring 0.5 h, violent
Under stirring condition, sodium borohydride aqueous solution is added drop-wise in the solution obtained by step (4)；Continue to stir 2.5 h after being added dropwise,
Filtering, after powder is cleaned with pure water, is dried in vacuo 30 h at 70 DEG C, obtains the modification galapectite nanometer of load Nanometer Copper
Pipe.
The remarkable advantage of the present invention：
On the one hand, because loading BaFe12O19Halloysite nanotubes have high magnetic loss angle tangent, can be with eddy-current loss, magnetic
The mechanism attenuation electromagnetic wave such as stagnant loss.In dielectric loss type nanocomposite A, the Nanometer Copper that average grain diameter is 2-6 nm is brilliant
Grain and the titanium dioxide nanoparticle that average grain diameter is 4-7 nm, are respectively provided with strong microwave attenuation characteristics.Dielectric loss type nanometer is answered
Average grain diameter is the nanometer titanium dioxide nickel particle of 3-6 nm in condensation material B, equally with strong microwave attenuation characteristics.Also, nanometer
Nickel dioxide, Nanometer Copper and nano-titanium dioxide possess different microwave attenuation mechanism and suction wavestrip is wide, can be mutual in performance
Collaboration supplement.What is more important, magnetic loss type nanocomposite, dielectric loss type nanocomposite A and dielectric loss
Type nanocomposite B uses halloysite nanotubes as load, and halloysite nanotubes are mainly by aluminium oxide and dioxy
SiClx forms, and the two is the material with strong microwave attenuation performance.The present invention will load BaFe12O19Halloysite nanotubes,
Dielectric loss type nanocomposite A, dielectric loss type nanocomposite B are combined, and preparing has electromagenetic wave radiation protection
The composite material of function, resulting materials have excellent microwave attenuation performance.
On the other hand, since the specific surface energy of above-mentioned nano material is high, large specific surface area easily agglomerates into block aggregation
Body and lose its excellent properties.For this purpose, the present invention carries out chemical modification to halloysite nanotubes, by overspending in its surface construction
Change macromolecular structure, to significantly increase the effect of the volume excluding between nano material.Meanwhile the present invention effectively divides in nano particle
On the basis of dissipating, load BaFe is coated using thermoplastic polypropylene12O19Halloysite nanotubes, dielectric loss type nanometer
Composite A and dielectric loss type nanocomposite B not only can effectively protect a variety of nano particles and keep its superiority
Can, and the composite material with electromagenetic wave radiation safeguard function formed can fully divide in the building materials system such as concrete
It dissipates, preferably plays the electromagenetic wave radiation protective benefits of composite material.Test shows provided by the present invention with electromagnetism amplitude
The composite material for penetrating safeguard function shows good broadband absorbing performance, and the bandwidth less than -7dB is 15.1GHz, less than -
The bandwidth of 10dB is 11.8GHz, can be applied to the electromagnetic wave proof of all kinds of key buildings.
Specific embodiment
Embodiment 1
Methacryloxypropyl trimethoxy silane used is commercially available, molecular weight：248.35 No. CAS：2530-
85-0, major product specification：Character：Colourless transparent liquid；Boiling point：190℃；198 °F of flash-point；Refractive index (25 DEG C)：
1.431；1.045 g/cm3 of density；Content：≥99%.
Halloysite nanotubes used be commercial product, main specifications：Character：White powder；Composition：SiO2：58.1、
Al2O3：41.02、TiO2：0.17、Fe2O3：0.38、P2O5：0.16；Bore：15-22 nm；Pipe outside diameter：40-70 nm；It is long
Degree：<1.5 μm；Specific surface area：53.4 m2/g；Density：2.5-2.6g/cm3。
γ used-(2,3- glycidoxy) propyl trimethoxy silicane is commercially available, chemical formula：C9H20O5Si, molecule
Amount：236.34 No. CAS:2530-83-8, major product specification：Character：Colourless transparent liquid；Boiling point：290℃；Refractive index
(25℃)：1.426-1.428；Density 1.07g/cm3；PH value：6.5-7；Content：≥98.0%.
Polysorbas20 used be commercial product, main specifications：Character：Pale yellow viscous liquid；Active matter：98-99%；
Acid value (KOHmg/g)：≤1.0；Hydroxyl value (KOHmg/g)：80-108；HLB value：16.7；Saponification number (KOHmg/g)：40-50；Water
Part (%)：≤1.0.
2- hydroxysuccinic acids used are commercial product, and CAS is numbered：6915-15-7, chemical formula：C4H6O5, molecular weight：
134.09 major product specification：Character：Colourless acicular crystal powder；Density (20 DEG C)：1.595 g/cm3；Fusing point：100
℃；Purity：≥99%；Decomposition point：140℃；Specific rotatory power：- 2.3 ° (8.5 grams/100 milliliters water)；Dissolubility：Soluble easily in water, second
Alcohol.
The preferably commercially available isotactic polypropylene of polypropylene used, major product specification：Density：1.12 g/cm3；Melt
Flow rate：6 g/10min（230 DEG C, 2.16 kg）；Heat distortion temperature：162 DEG C (0.45 Mpa, unannealed)；Tensile strength：
105 Mpa；IZOD impact strengths：10 J/m（It is 23 DEG C 1/4 " thick）；Bending strength：145 Mpa；Identation hardness：125 Mpa.
Boron trifluoride etherate used is commercial product, and CAS is numbered：109-63-7, chemical formula：C4H10BF3O,
Molecular weight：141.93 major product specification：Character：Colourless liquid；Fusing point：−58℃；Boiling point：126-129 ℃；Density：
1.15 g/mL；Purity：It analyzes pure；Content of beary metal：≤10 ppm.
Diallyl dimethyl ammoniumchloride used is commercially available, No. CAS:26062-79-3, major product specification：
Character：Colourless viscous liquid；Solidification point is -2.8 DEG C；Density is 1.04g/cm3；286 DEG C of decomposition temperature；Dissolubility：It is soluble in
Water.
Poly- naphthalene formaldehyde sulfonate used is commercial product, and CAS is numbered：9084-06-4, chemical formula (C11H7O4SNa) n,
Its main specifications：Character：Brown ceramic powder；Dissolubility：It is soluble easily in water.
Copper dichloride dihydrate used, barium nitrate, titanium tetrachloride, potassium chloride, ammonium sulfate, six hydration Nickel Chlorides, nitric acid
Iron (III) nonahydrate, ammonium hydroxide, absolute ethyl alcohol, 3- methyl -3- oxetane methanols and chloroform are that commercially available chemistry is pure
Product.
Embodiment 1
1. the activating treatment method of pair halloysite nanotubes：
（1）Halloysite nanotubes are taken, it is for use after mechanical crushing is handled and 350 mesh sieves is used to select；
（2）Respectively be packed into two 6 identical L nylon tanks 50 a diameter of 5 mm stainless steel ball and 40 it is a diameter of
The stainless steel ball of 10 mm, is then respectively adding step（1）2.6 kg of halloysite nanotubes, then that 360 ml are added dropwise respectively is anhydrous
Ethyl alcohol, and sealed with nylon lid.Two ball grinders are symmetrically put into planetary ball mill, are 350 rpm and every in rotating speed
Under conditions of 30 minutes automatic conversion direction of rotation after 50 h of ball milling, the chopped galapectite nanometer that length is 210-240 nm is obtained
Pipe；
（3）By step（2）The gained halloysite nanotubes that are chopped are added to 20 water of Tween that pH is 8, concentration is 15 wt%
24 h of ultrasound in solution, filtering, after being eluted with water, are dried in vacuo after 30 h to get the Ai Luo of activated processing at 68-70 DEG C
Stone nanotube.
2. the halloysite nanotubes that surface is modified：
By 3.2 kg of halloysite nanotubes of activated processing, it is added in 46 L chloroforms, under nitrogen protection room
After temperature is ultrasonically treated 5 h, adds in 122 ml boron trifluoride etherates and 4.5 h are stirred at room temperature；It -10 ~ 12 DEG C and is stirring again
Under the conditions of mixing, 610 ml 3- methyl -3- oxetane methanols are slowly added dropwise in the 8 h times of control, are added dropwise after -9 ~ 11
DEG C continue to stir 24 h；Then 900 ml absolute ethyl alcohols are added in, by 0.5 h of rotating speed centrifugal treating of 5000-5300 rpm, separation
Recycling design, powder are cleaned through absolute ethyl alcohol, and are dried in vacuo 20 h at room temperature, obtain the modification of 3.47-3.61 kg surfaces
Halloysite nanotubes.
3. load BaFe12O19Halloysite nanotubes：
（1）At 20-22 DEG C, 20.41 parts of ferric nitrate (III) nonahydrates and 1.1 parts of barium nitrates are added to 150 parts
It is for use after 2 h of stirring in ionized water；
（2）At 28-30 DEG C and under stirring, by 15.1 parts of 2- hydroxy propanes -1,2,3- tricarboxylic acids is added dropwise to the water of step (1)
In solution, time for adding is 0.5 h；Continue to be placed at room temperature for for use after stirring 3 h after being added dropwise；
（3）The ammonium hydroxide that 6.1 parts of concentration are 20 % is added dropwise in the solution of step (2), time for adding is 1 h；
（4）The halloysite nanotubes of 3.3 parts of activated processing are added in the solution of step (3), it is acute after 2 h of ultrasound
1 h of strong stirring then heats to 87-88 DEG C, and room temperature is for use after stirring 5.5 h.
（5）After the mixture of step (4) is handled 4.5 h at 123-125 DEG C, continue to handle 4 at 855-857 DEG C
H obtains load BaFe12O19Halloysite nanotubes.
4. load the modification halloysite nanotubes of Nanometer Copper:
（1）Under the gentle agitation of room, 7.15 parts of potassium chloride are added in 50 parts of deionized waters, continue to treat after stirring 1.5 h
With；
（2）It adds in 2.89 parts of surfaces and is modified halloysite nanotubes, after stirring 2 h, then 2 h of ultrasound, then add in 7.53 parts
Diallyl dimethyl ammoniumchloride filters after being vigorously stirred 6 h, for use after powder is cleaned with pure water；
（3）Under the gentle agitation of room, 9.4 parts of poly- naphthalene formaldehyde sulfonates are added in 25 parts of deionized waters, stir 5 h
Afterwards, add in the powder that step (2) is got ready, filtered after being vigorously stirred 5 h, by powder pure water cleaned standby seam；
（4）Under the gentle agitation of room, by 1.2 parts of 2- hydroxysuccinic acids and 6.25 parts of alkylphenol polyoxyethylene ether and step
(3) powder got ready is added in deionized water simultaneously, is continued after stirring 1.5 h, is added in 1.62 parts of Copper dichloride dihydrates, acute
4 h of ultrasound after 1 h of strong stirring, obtain solution for later use；
（5）At 1-3 DEG C, 7.35 parts of sodium borohydrides are added in 28 parts of deionized waters, after stirring 0.5 h, violent
Under stirring condition, sodium borohydride aqueous solution is added drop-wise in the solution obtained by step (4)；Continue to stir 2.5 h after being added dropwise,
Filtering, after powder is cleaned with pure water, is dried in vacuo 30 h at 70 DEG C, obtains the modification galapectite nanometer of load Nanometer Copper
Pipe.
5. dielectric loss type nanocomposite A:
（1）Under room temperature and stirring condition, 0.5 part of alkylphenol polyoxyethylene ether and 0.65 part of ammonium sulfate are added to 22 parts
It is for use after 3 h of stirring in ionized water；
（2）The modification halloysite nanotubes of 1.6 parts of load Nanometer Coppers are added in, after stirring 2 h, then 1 h of ultrasound, it is cooled to 1-
3 DEG C for use；
（3）0.85 part of titanium tetrachloride is added, is vigorously stirred 3 h；23-25 DEG C is then heated to, continues to be vigorously stirred 1.5
After h, ammonium hydroxide is added dropwise, time for adding is 1 h；Continue to stir 0.5 h after being added dropwise, filter, after powder is cleaned with pure water,
24 h are dried in vacuo at 65 DEG C, obtain dielectric loss type nanocomposite A.
6. dielectric loss type nanocomposite B：
（1）Under the gentle agitation of room, 5.4 parts of sodium chloride are added in 28 parts of deionized waters, continue to stir for use after 1 h；
（2）The halloysite nanotubes that 1.95 parts of surfaces are modified are added in the aqueous solution of step (1), are vigorously stirred 2 h
Afterwards, then 1 h of ultrasound, 6.2 parts of dimethyl diallyl ammonium chloride-acrylamide copolymers are then added in, are vigorously stirred mistake after 2 h
Filter, it is for use after powder is cleaned with pure water；
（3）Under the gentle agitation of room, 5.85 parts of kayexalates are added in 16 parts of deionized waters, continue to stir
After 2 h, the powder that step (2) is got ready is added in, filters, powder is cleaned with pure water, for use after being vigorously stirred 2.5 h；
（4）The powder of step (3) is added in 17 parts of deionized waters, after stirring 2 h, adds in 6.2 parts of dimethyl diene
Propyl ammonium chloride-acrylamide copolymer filters after being vigorously stirred 3 h, for use after powder is cleaned with pure water；
（5）Under the gentle agitation of room, the powder of step (4) and 3.0 parts of octyl phenol polyoxyethylene ether are added to 22 simultaneously
In part deionized water, continue after stirring 2 h, add in 103 parts of 2- hydroxy propanes -1,2,3- tricarboxylic acids simultaneously stirs 0.5 h, Ran Houjia
Enter 1.5 part of six hydration Nickel Chloride, be vigorously stirred 3 h, then be cooled to 1-3 DEG C, obtain solution for later use；
（6）At 1-3 DEG C, 5.8 parts of sodium borohydrides are added in 20 parts of ionized waters, after stirring 15 min, at 1-3 DEG C and
It is vigorously stirred down, is added drop-wise in the solution of step (5), time for adding is 1 h；It is filtered after being added dropwise, powder is washed with pure water
After net, 30 h are dried in vacuo at 70 DEG C, obtain dielectric loss type nanocomposite B.
7. the preparation of the composite material with electromagenetic wave radiation safeguard function：
(1) BaFe is loaded by 2 parts12O19Halloysite nanotubes and 0.6 part of methacryloxypropyl trimethoxy
After 3 h are stirred at room temperature in silane, 12 parts of polypropylene are added in, the mixed of the nanocomposite containing magnetic loss type is formed after stirring 3 h
Material is closed, for use；
(2) at room temperature, 1.3 parts of dielectric loss type nanocomposite A are taken, 0.6 part of γ-(2,3- the third oxygen of epoxy are added dropwise
Base) propyl trimethoxy silicane, after stirring 1 h, add in 20 parts of polypropylene and stir 1.5 h；Add 1.2 parts of dielectric loss types
0.2 part of γ-(2,3- glycidoxy) propyl trimethoxy silicane is added dropwise in nanocomposite B, after stirring 1 h, with step
(1) mixture got ready is fitted into high-speed mixer simultaneously, and 3 h are disperseed under 350 r/min rotating speeds；115 DEG C are then heated to,
It after handling 24 min under 550 r/min rotating speeds, is transferred in cold mixing pot, blowing obtains just batch mixing when temperature is down to 52 DEG C；
(3) the first batch mixing that step (2) prepares is placed in the twin-screw that temperature is 180 DEG C, rotating speed is 80 r/min to squeeze
Go out in machine after being kneaded 1.5 h and squeeze out, obtain mixing materials；
(4) the mixing materials pulverization process for preparing above-mentioned steps (3) has electromagenetic wave radiation protection to get to one kind
The composite material of function, granularity are 220 mesh.
Embodiment 2
Halloysite nanotubes, the load BaFe of activating treatment method and surface modification to halloysite nanotubes12O19
Halloysite nanotubes, dielectric loss type nanocomposite B, load Nanometer Copper modification halloysite nanotubes and dielectric loss
The preparation of type nanocomposite A is the same as described in embodiment 1.On this basis, answering with electromagenetic wave radiation safeguard function is prepared
Condensation material：
(1) BaFe is loaded by 1.5 parts12O19Halloysite nanotubes and 0.4 part of methacryloxypropyl trimethoxy
After 3 h are stirred at room temperature in base silane, 12 parts of polypropylene are added in, the nanocomposite containing magnetic loss type is formed after stirring 3 h
Mixture, for use；
(2) at room temperature, 0.9 part of dielectric loss type nanocomposite A is taken, 0.3 part of γ-(2,3- the third oxygen of epoxy are added dropwise
Base) propyl trimethoxy silicane, after stirring 1 h, add in 10 parts of polypropylene and stir 1.5 h；Add 0.8 part of dielectric loss
0.2 part of γ-(2,3- glycidoxy) propyl trimethoxy silicane is added dropwise in type nanocomposite B, after stirring 1 h, with step
(1) mixture got ready is fitted into high-speed mixer simultaneously, and 2.5 h are disperseed under 300 r/min rotating speeds；Then heat to 112
DEG C, it after handling 20 min under 450 r/min rotating speeds, is transferred in cold mixing pot, blowing obtains just batch mixing when temperature is down to 55 DEG C；
(3) the first batch mixing that step (2) prepares is placed in the twin-screw that temperature is 170 DEG C, rotating speed is 70 r/min to squeeze
Go out in machine after being kneaded 1 h and squeeze out, obtain mixing materials；
(4) the mixing materials pulverization process for preparing step (3) has electromagenetic wave radiation safeguard function to get to one kind
Composite material, granularity be 160 mesh.
Embodiment 3
Halloysite nanotubes, the load BaFe of activating treatment method and surface modification to halloysite nanotubes12O19
Halloysite nanotubes, dielectric loss type nanocomposite B, load Nanometer Copper modification halloysite nanotubes and dielectric loss
The preparation of type nanocomposite A is the same as embodiment 1.On this basis, the composite wood with electromagenetic wave radiation safeguard function is prepared
Material：
(1) BaFe is loaded by 1.7 parts12O19Halloysite nanotubes and 0.5 part of methacryloxypropyl trimethoxy
After 3 h are stirred at room temperature in base silane, 12 parts of polypropylene are added in, the nanocomposite containing magnetic loss type is formed after stirring 3 h
Mixture, for use；
(2) at room temperature, 1.2 parts of dielectric loss type nanocomposite A are taken, 0.4 part of γ-(2,3- the third oxygen of epoxy are added dropwise
Base) propyl trimethoxy silicane, after stirring 1 h, add in 13 parts of polypropylene and stir 1.5 h；Add 1.1 parts of dielectric loss types
0.2 part of γ-(2,3- glycidoxy) propyl trimethoxy silicane is added dropwise in nanocomposite B, after stirring 1 h, with step
(1) mixture got ready is fitted into high-speed mixer simultaneously, and 2 h are disperseed under 320 r/min rotating speeds；115 DEG C are then heated to,
It after handling 22 min under 520 r/min rotating speeds, is transferred in cold mixing pot, blowing obtains just batch mixing when temperature is down to 50 DEG C；
(3) the first batch mixing that step (2) prepares is placed in the twin-screw that temperature is 175 DEG C, rotating speed is 75 r/min to squeeze
Go out in machine after being kneaded 1 h and squeeze out, obtain mixing materials；
(4) the mixing materials pulverization process for preparing step (3) has electromagenetic wave radiation safeguard function to get to one kind
Composite material, granularity be 200 mesh.
Composite material obtained by above-described embodiment is respectively provided with good microwave attenuation performance.
The foregoing is merely presently preferred embodiments of the present invention, all equivalent changes done according to scope of the present invention patent with
Modification should all belong to the covering scope of the present invention.
Claims (9)
1. a kind of composite material with electromagenetic wave radiation safeguard function, it is characterised in that：Each component raw material is according to following weight
Part composition：A, 1.5-2 parts of load BaFe of 0.9-1.3 parts of dielectric loss type nanocomposites12O19Halloysite nanotubes,
0.4-0.6 parts of methacryloxypropyl trimethoxy silanes, 0.8-1.2 parts of dielectric loss type nanocomposites B, 0.5-
0.8 part of γ-(2,3- glycidoxies) propyl trimethoxy silicane, 22-32 parts of polypropylene；Its dielectric loss type is nano combined
Contain Nanometer Copper crystal grain and titanium dioxide nanoparticle in materials A；Contain nano-silica in dielectric loss type nanocomposite B
Change nickel particle.
2. the composite material according to claim 1 with electromagenetic wave radiation safeguard function, it is characterised in that：The dielectric
Loss-type nanocomposite A is made by following steps：
（1）Under room temperature and stirring condition, 0.5 part of alkylphenol polyoxyethylene ether and 0.65 part of ammonium sulfate are added to 22 parts of deionizations
It is for use after 3 h of stirring in water；
（2）The modification halloysite nanotubes of 1.6 parts of load Nanometer Coppers are added in, after stirring 2 h, then 1 h of ultrasound, it is cooled to 1-3 DEG C
For use；
（3）0.85 part of titanium tetrachloride is added, is vigorously stirred 3 h；23-25 DEG C is then heated to, continues to be vigorously stirred 1.5 h
Afterwards, ammonium hydroxide is added dropwise, time for adding is 1 h；Continue to stir 0.5 h after being added dropwise, filter, after powder is cleaned with pure water,
24 h are dried in vacuo at 65 DEG C, obtain dielectric loss type nanocomposite A.
3. the composite material according to claim 2 with electromagenetic wave radiation safeguard function, it is characterised in that：The load
The modification halloysite nanotubes of Nanometer Copper are made by following steps：
（1）Under the gentle agitation of room, 7.15 parts of potassium chloride are added in 50 parts of deionized waters, continue to stir for use after 1.5 h；
（2）It adds in 2.89 parts of surfaces and is modified halloysite nanotubes, after stirring 2 h, then 2 h of ultrasound, then add in 7.53 parts poly- two
Allyl dimethyl ammonium chloride filters after being vigorously stirred 6 h, for use after powder is cleaned with pure water；
（3）Under the gentle agitation of room, 9.4 parts of poly- naphthalene formaldehyde sulfonates are added in 25 parts of deionized waters, after stirring 5 h, are added
Enter in the powder that step (2) is got ready, filtered after being vigorously stirred 5 h, by powder pure water cleaned standby seam；
（4）It is under the gentle agitation of room, 1.2 parts of 2- hydroxysuccinic acids and 6.25 parts of alkylphenol polyoxyethylene ether and step (3) are standby
Good powder is added to simultaneously in deionized water, is continued after stirring 1.5 h, is added in 1.62 parts of Copper dichloride dihydrates, acutely stir
4 h of ultrasound after 1 h are mixed, obtain solution for later use；
（5）At 1-3 DEG C, 7.35 parts of sodium borohydrides are added in 28 parts of deionized waters, after stirring 0.5 h, are being vigorously stirred
Under the conditions of, sodium borohydride aqueous solution is added drop-wise in the solution obtained by step (4)；Continue to stir 2.5 h, mistake after being added dropwise
Filter, after powder is cleaned with pure water, is dried in vacuo 30 h at 70 DEG C, obtains the modification halloysite nanotubes of load Nanometer Copper.
4. the composite material according to claim 1 with electromagenetic wave radiation safeguard function, it is characterised in that：Load
BaFe12O19Halloysite nanotubes be made by following steps：
（1）At 20-22 DEG C, 20.41 parts of ferric nitrate (III) nonahydrates and 1.1 parts of barium nitrates are added to 150 parts of deionizations
It is for use after 2 h of stirring in water；
（2）At 28-30 DEG C and under stirring, by 15.1 parts of 2- hydroxy propanes -1,2,3- tricarboxylic acids is added dropwise to the aqueous solution of step (1)
In, time for adding is 0.5 h；Continue to be placed at room temperature for for use after stirring 3 h after being added dropwise；
（3）The ammonium hydroxide that 6.1 parts of concentration are 20 % is added dropwise in the solution of step (2), time for adding is 1 h；
（4）The halloysite nanotubes of 3.3 parts of activated processing are added in the solution of step (3), after 2 h of ultrasound, acutely stirred
1 h is mixed, then heats to 87-88 DEG C, room temperature is for use after stirring 5.5 h；
（5）After the mixture of step (4) is handled 4.5 h at 123-125 DEG C, continue to handle 4 h at 855-857 DEG C, obtain
To load BaFe12O19Halloysite nanotubes.
5. the composite material according to claim 1 with electromagenetic wave radiation safeguard function, it is characterised in that：The dielectric
Loss-type nanocomposite B is made by following steps：
（1）Under the gentle agitation of room, 5.4 parts of sodium chloride are added in 28 parts of deionized waters, continue to stir for use after 1 h；
（2）The halloysite nanotubes that 1.95 parts of surfaces are modified are added in the aqueous solution of step (1), after being vigorously stirred 2 h, then
Then 1 h of ultrasound adds in 6.2 parts of dimethyl diallyl ammonium chloride-acrylamide copolymers, is filtered after being vigorously stirred 2 h, will
Powder is for use after being cleaned with pure water；
（3）Under the gentle agitation of room, 5.85 parts of kayexalates are added in 16 parts of deionized waters, continue to stir 2 h
Afterwards, the powder that step (2) is got ready is added in, filters, powder is cleaned with pure water, for use after being vigorously stirred 2.5 h；
（4）The powder of step (3) is added in 17 parts of deionized waters, after stirring 2 h, adds in 6.2 parts of dimethyl diallyls
Ammonium chloride-acrylamide copolymer filters after being vigorously stirred 3 h, for use after powder is cleaned with pure water；
（5）Under the gentle agitation of room, the powder of step (4) and 3.0 parts of octyl phenol polyoxyethylene ether are added to 22 parts simultaneously
In ionized water, continue after stirring 2 h, add in 103 parts of 2- hydroxy propanes -1,2,3- tricarboxylic acids simultaneously stirs 0.5 h, then adds in
1.5 part of six hydration Nickel Chloride, is vigorously stirred 3 h, then is cooled to 1-3 DEG C, obtains solution for later use；
（6）At 1-3 DEG C, 5.8 parts of sodium borohydrides are added in 20 parts of ionized waters, after stirring 15 min, at 1-3 DEG C and acutely
It under stirring, is added drop-wise in the solution of step (5), time for adding is 1 h；It is filtered after being added dropwise, after powder is cleaned with pure water,
30 h are dried in vacuo at 70 DEG C, obtain dielectric loss type nanocomposite B.
6. the composite material with electromagenetic wave radiation safeguard function according to claim 3 or 5, it is characterised in that：It is described
Surface is modified halloysite nanotubes and comprises the following steps：
By 3.2 kg of halloysite nanotubes of activated processing, it is added in 46 L chloroforms, room temperature surpasses under nitrogen protection
After 5 h of sonication, add in 122 ml boron trifluoride etherates and 4.5 h are stirred at room temperature；Again in -10 ~ 12 DEG C and stirring bar
Under part, control 8 h times 610 ml 3- methyl -3- oxetane methanols are slowly added dropwise, be added dropwise after -9 ~ 11 DEG C after
24 h of continuous stirring；Then 900 ml absolute ethyl alcohols are added in, by 0.5 h of rotating speed centrifugal treating of 5000-5300 rpm, separation and recovery
Solvent, powder are cleaned through absolute ethyl alcohol, and are dried in vacuo 20 h at room temperature, obtain the Ai Luo of 3.47-3.61 kg surfaces modification
Stone nanotube.
7. the composite material according to claim 6 with electromagenetic wave radiation safeguard function, it is characterised in that：It is described through work
Change comprising the following steps for the halloysite nanotubes of processing：
（1）Halloysite nanotubes are taken, it is for use after mechanical crushing is handled and 350 mesh sieves is used to select；
（2）The stainless steel ball and 40 a diameter of 10 mm of 50 a diameter of 5 mm are respectively packed into two 6 identical L nylon tanks
Stainless steel ball, be then respectively adding step（1）2.6 kg of halloysite nanotubes, then 360 ml absolute ethyl alcohols are added dropwise respectively,
And it is sealed with nylon lid；Two ball grinders are symmetrically put into planetary ball mill, are 350 rpm and 30 points every in rotating speed
Under conditions of clock automatic conversion direction of rotation after 50 h of ball milling, the chopped halloysite nanotubes that length is 210-240 nm are obtained；
（3）By step（2）The gained halloysite nanotubes that are chopped are added to 20 aqueous solutions of Tween that pH is 8, concentration is 15 wt%
Middle ultrasonic 24 h, filtering, after being eluted with water, is dried in vacuo after 30 h at 68-70 DEG C and is received to get the galapectite of activated processing
Mitron.
8. a kind of preparation method of the composite material as described in claim 1 with electromagenetic wave radiation safeguard function, feature
It is：Specifically comprise the following steps：
（1）BaFe will be loaded12O19Halloysite nanotubes and methacryloxypropyl trimethoxy silane stir at room temperature
After mixing, polypropylene is added in, the mixture of the nanocomposite containing magnetic loss type is formed after stirring, for use；
（2）At room temperature, dielectric loss type nanocomposite A is taken, γ-(2,3- glycidoxy) propyl trimethoxy is added dropwise
Silane, after stirring, after adding in polypropylene and stirring；Dielectric loss type nanocomposite B is added, γ-(2,3- epoxies are added dropwise
Propoxyl group) propyl trimethoxy silicane, after stirring, it is fitted into high-speed mixer and disperses simultaneously with the mixture obtained by step (1)；
Then after heating stirring, it is transferred to blowing after cooling down in cold mixing pot and obtains just batch mixing；
（3）By first batch mixing mixing extrusion obtained by step (2), mixing materials are obtained；
（4）By mixing materials pulverization process obtained by step (3) to get to the composite material with electromagenetic wave radiation safeguard function.
9. preparation method according to claim 8, it is characterised in that：Step（3）Described in mixing extrusion condition be：Temperature
It is 70-80 r/min to spend for 170-180 DEG C, rotating speed.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5660772A (en) * | 1993-09-27 | 1997-08-26 | Alfred University | Process for making ultra-fine barium hexaferrite particles |
| CN103224595A (en) * | 2013-04-16 | 2013-07-31 | 山东建筑大学 | Polymer-based absorbing nanomaterial |
| CN104130458A (en) * | 2014-07-24 | 2014-11-05 | 中国热带农业科学院农产品加工研究所 | Absorbing material and preparation method |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5660772A (en) * | 1993-09-27 | 1997-08-26 | Alfred University | Process for making ultra-fine barium hexaferrite particles |
| CN103224595A (en) * | 2013-04-16 | 2013-07-31 | 山东建筑大学 | Polymer-based absorbing nanomaterial |
| CN104130458A (en) * | 2014-07-24 | 2014-11-05 | 中国热带农业科学院农产品加工研究所 | Absorbing material and preparation method |
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