CN109796729A - A kind of nano combined absorbing material and preparation method thereof - Google Patents
A kind of nano combined absorbing material and preparation method thereof Download PDFInfo
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- CN109796729A CN109796729A CN201910128250.6A CN201910128250A CN109796729A CN 109796729 A CN109796729 A CN 109796729A CN 201910128250 A CN201910128250 A CN 201910128250A CN 109796729 A CN109796729 A CN 109796729A
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Abstract
The present invention provides a kind of nano combined absorbing materials and preparation method thereof, it is prepared by the raw material of following parts by weight: 40-60 parts of epoxy resin E-44, 12-20 parts of nano-graphene, 10-18 parts of magnetic nanometer, 8-15 parts of nano-titanium dioxide, 7-16 parts of nano zine oxide, 5-10 parts of nanometer cobalt oxide, 6-12 parts of nano tungsten trioxide, 4-9 parts of gamma-aminopropyl-triethoxy-silane, 3-8 parts of toluene di-isocyanate(TDI), 2-5 parts of carbothioic acid allyl amide of benzotriazole -1-, 3-7 parts of butylene terephthalate, 1-5 parts of neopelex, 2-6 parts of polybutylene terephthalate (PBT), 4-7 parts of polyamide, 20-40 parts of isopropanol, 10-20 parts of acetone.Wave suction composite material wave absorbing efficiency prepared by the present invention is high, absorbing property is good, therefore nano wave-absorbing material produced by the present invention has a good application prospect.
Description
Technical field
The invention belongs to technical field of electronic materials, and in particular to a kind of nano combined absorbing material and preparation method thereof.
Background technique
Absorbing material be refer to absorb, the energy of decaying incident electromagnetic wave, directly electro-magnetic wave absorption can be fallen and not
Generate vortex, not reflection electromagnetic wave does not cause secondary pollution to the electronic component of surrounding, and by the dielectric loss of material or
Magnetic loss makes electromagnetic energy be quickly converted into thermal energy or a kind of new function material of other form of energy.With various electronic equipments
Frequent use, electromagnetic radiation and electromagnetic pollution are got worse.The development and exploitation of electromagnetic-wave absorbent increasingly cause people
Concern, novel absorbing material emerges one after another.
Traditional magnetic material as wave absorbing agent in use, have many advantages, such as to absorb that strong, frequency band is wider and at low cost, but it is same
When the disadvantages of that there are density is big, poor mechanical property, novel absorbing material is required to meet the feature of " thin, light, wide, strong ", and not
Stealthy multiple spectra, environment adaptation, high temperature resistant, shock resistance, Antiradiation, marine climate resistant should then be reached by carrying out ideal absorbing material
Etc. requirements at the higher level.Therefore, while being further improved to traditional absorbing material, various novel wave-absorbing materials is explored, are current
The research hotspot and emphasis in the field.
Summary of the invention
Above of the existing technology in order to solve the problems, such as, the purpose of the present invention is to provide a kind of nano combined suction wave materials
Material and preparation method thereof.
To achieve the goals above, the present invention the following technical schemes are provided:
A kind of nano combined absorbing material, is prepared by the raw material of following parts by weight: 40-60 parts of epoxy resin E-44,
12-20 parts of nano-graphene, 10-18 parts of magnetic nanometer, 8-15 parts of nano-titanium dioxide, 7-16 parts of nano zine oxide, nanometer
5-10 parts of cobalt oxide, 6-12 parts of nano tungsten trioxide, 4-9 parts of gamma-aminopropyl-triethoxy-silane, toluene di-isocyanate(TDI) 3-8
Part, 2-5 parts of benzotriazole -1- carbothioic acid allyl amide, 3-7 parts of butylene terephthalate, neopelex
1-5 parts, 2-6 parts of polybutylene terephthalate (PBT), 4-7 parts of polyamide, 20-40 parts of isopropanol, 10-20 parts of acetone.
Further, a kind of nano combined absorbing material of the present invention, is prepared by the raw material of following parts by weight:
50 parts of epoxy resin E-44,16 parts of nano-graphene, 14 parts of magnetic nanometer, 12 parts of nano-titanium dioxide, nano zine oxide 11
Part, 8 parts of nanometer cobalt oxide, 9 parts of nano tungsten trioxide, 7 parts of gamma-aminopropyl-triethoxy-silane, 6 parts of toluene di-isocyanate(TDI),
3.5 parts of benzotriazole -1- carbothioic acid allyl amide, 3 parts of neopelex, gathers at 5 parts of butylene terephthalate
4 parts of mutual-phenenyl two acid bromide two alcohol ester, 5.5 parts of polyamide, 30 parts of isopropanol, 15 parts of acetone.
Further, in a kind of nano combined absorbing material of the present invention, the epoxide number of the epoxy resin E-44
For 0.42-0.46mol/100g, dielectric constant 3.0-3.4.
A kind of preparation method of nano combined absorbing material of the present invention, preparation step are as follows:
(1) by nano-graphene, magnetic nanometer, nano-titanium dioxide, nano zine oxide, nanometer cobalt oxide, nanometer three
Tungsten oxide, gamma-aminopropyl-triethoxy-silane are added in agitator tank, and isopropanol is then added and is stirred 20-40min, in
Continue to stir 1-2h under the conditions of 35-50 DEG C of temperature, mixture A is made；
(2) epoxy resin E-44 is added in acetone soln and is dissolved, is then added under stirring conditions
To into mixture A made from step (1), after stirring 10-20min, toluene diisocynate is sequentially added under stirring conditions
Ester, benzotriazole -1- carbothioic acid allyl amide, butylene terephthalate, neopelex, poly- terephthaldehyde
Sour butanediol ester and polyamide continue to stir 2-4h under the conditions of 40-50 DEG C of temperature, mixture B are made；
(3) mixture B is placed on mixer, mixing 30-50min is carried out at 130-160 DEG C, after standing 10-20h,
It is placed on mixer again, carries out being kneaded 20-40min discharging at 160-200 DEG C, obtain rubber compound；
(4) above-mentioned rubber compound is placed on calender, with 90-120kg.cm-2Pressure, under the conditions of 120-150 DEG C of temperature
Calendering is in flakes to get nano combined absorbing material.
Further, the preparation method of a kind of nano combined absorbing material of the present invention, in the preparation process
Speed of agitator is 200-600r/min.
The utility model has the advantages that the present invention provides a kind of nano combined absorbing material and preparation method thereof, suction prepared by the present invention
Wave composite material is under 3mm thickness, and minimum reflectance is between -17.2~-18.6dB, effective Absorber Bandwidth (< -10dB)
Up to 6.5~8.3GHz, wave absorbing efficiency is high, and also shows absorbing property in low-frequency range, and absorbing property is good, therefore the present invention is made
Nano wave-absorbing material have a good application prospect.
Specific embodiment
Combined with specific embodiments below, present invention is further described in detail.The following examples are intended to illustrate the invention,
But it is not intended to limit the scope of the invention.
Embodiment 1
A kind of nano combined absorbing material, is prepared by the raw material of following parts by weight: 50 parts of epoxy resin E-44 is received
16 parts of graphene of rice, 12 parts of nano-titanium dioxide, 11 parts of nano zine oxide, 8 parts of nanometer cobalt oxide, is received 14 parts of magnetic nanometer
Rice 9 parts of tungstic acid, 7 parts of gamma-aminopropyl-triethoxy-silane, 6 parts of toluene di-isocyanate(TDI), benzotriazole -1- carbothioic acid
3.5 parts of allyl amide, 5 parts of butylene terephthalate, 3 parts of neopelex, polybutylene terephthalate (PBT) 4
Part, 5.5 parts of polyamide, 30 parts of isopropanol, 15 parts of acetone.
The epoxide number of the epoxy resin E-44 is 0.44mol/100g, dielectric constant 3.2.
A kind of preparation method of nano combined absorbing material of the present invention, preparation step are as follows:
(1) by nano-graphene, magnetic nanometer, nano-titanium dioxide, nano zine oxide, nanometer cobalt oxide, nanometer three
Tungsten oxide, gamma-aminopropyl-triethoxy-silane are added in agitator tank, and isopropanol is then added and is stirred 30min, in 42 DEG C
Temperature under the conditions of continue stir 1.5h, be made mixture A；
(2) epoxy resin E-44 is added in acetone soln and is dissolved, is then added under stirring conditions
To into mixture A made from step (1), after stirring 15min, sequentially add under stirring conditions toluene di-isocyanate(TDI),
Benzotriazole -1- carbothioic acid allyl amide, butylene terephthalate, neopelex, poly terephthalic acid
Butanediol ester and polyamide continue to stir 3h under the conditions of 45 DEG C of temperature, mixture B are made；
(3) mixture B is placed on mixer, mixing 40min is carried out at 145 DEG C, after standing 15h, then be placed in mixing
On machine, carries out being kneaded 30min discharging at 180 DEG C, obtain rubber compound；
(4) above-mentioned rubber compound is placed on calender, with 105kg.cm-2Pressure, the pushing of 135 DEG C of temperature conditions prolongs into
Piece is to get nano combined absorbing material.
A kind of preparation method of nano combined absorbing material of the present invention, the speed of agitator in the preparation process are
400r/min。
Embodiment 2
A kind of nano combined absorbing material, is prepared by the raw material of following parts by weight: 40 parts of epoxy resin E-44 is received
Rice 12 parts of graphene, 10 parts of magnetic nanometer, 8 parts of nano-titanium dioxide, 7 parts of nano zine oxide, nanometer cobalt oxide 5 part, nanometer
6 parts of tungstic acid, 4 parts of gamma-aminopropyl-triethoxy-silane, 3 parts of toluene di-isocyanate(TDI), benzotriazole -1- carbothioic acid alkene
2 parts of propyl amides, 3 parts of butylene terephthalate, 1 part of neopelex, 2 parts of polybutylene terephthalate (PBT),
4 parts of polyamide, 20 parts of isopropanol, 10 parts of acetone.
The epoxide number of the epoxy resin E-44 is 0.42mol/100g, dielectric constant 3.0.
A kind of preparation method of nano combined absorbing material of the present invention, preparation step are as follows:
(1) by nano-graphene, magnetic nanometer, nano-titanium dioxide, nano zine oxide, nanometer cobalt oxide, nanometer three
Tungsten oxide, gamma-aminopropyl-triethoxy-silane are added in agitator tank, and isopropanol is then added and is stirred 20min, in 35 DEG C
Temperature under the conditions of continue stir 1h, be made mixture A；
(2) epoxy resin E-44 is added in acetone soln and is dissolved, is then added under stirring conditions
To into mixture A made from step (1), after stirring 10min, sequentially add under stirring conditions toluene di-isocyanate(TDI),
Benzotriazole -1- carbothioic acid allyl amide, butylene terephthalate, neopelex, poly terephthalic acid
Butanediol ester and polyamide continue to stir 2h under the conditions of 40 DEG C of temperature, mixture B are made；
(3) mixture B is placed on mixer, mixing 30min is carried out at 130 DEG C, after standing 10h, then be placed in mixing
On machine, carries out being kneaded 20min discharging at 160 DEG C, obtain rubber compound；
(4) above-mentioned rubber compound is placed on calender, with 90kg.cm-2Pressure, the pushing of 120 DEG C of temperature conditions prolongs in flakes,
Up to nano combined absorbing material.
Speed of agitator in the preparation process is 200r/min.
Embodiment 2
A kind of nano combined absorbing material, is prepared by the raw material of following parts by weight: epoxy resin E-44 45 part, nanometer
15 parts of graphene, 12 parts of magnetic nanometer, 10 parts of nanometer titanium dioxide, 9 parts of nano zine oxide, 6 three oxygen of part, nanometer of nanometer cobalt oxide
Change 7 parts of tungsten, 5 parts of gamma-aminopropyl-triethoxy-silane, 5 parts of toluene di-isocyanate(TDI), benzotriazole -1- carbothioic acid allyl
3 parts of amide, 4 parts of butylene terephthalate, 2 parts of neopelex, 3 parts of polybutylene terephthalate (PBT), polyamides
5 parts of amine, 25 parts of isopropanol, 12 parts of acetone.
The epoxide number of the epoxy resin E-44 is 0.423mol/100g, dielectric constant 3.1.
A kind of preparation method of nano combined absorbing material of the present invention, preparation step are as follows:
(1) by nano-graphene, magnetic nanometer, nano-titanium dioxide, nano zine oxide, nanometer cobalt oxide, nanometer three
Tungsten oxide, gamma-aminopropyl-triethoxy-silane are added in agitator tank, and isopropanol is then added and is stirred 25min, in 40 DEG C
Temperature under the conditions of continue stir 1.2h, be made mixture A；
(2) epoxy resin E-44 is added in acetone soln and is dissolved, is then added under stirring conditions
To into mixture A made from step (1), after stirring 12min, sequentially add under stirring conditions toluene di-isocyanate(TDI),
Benzotriazole -1- carbothioic acid allyl amide, butylene terephthalate, neopelex, poly terephthalic acid
Butanediol ester and polyamide continue to stir 2.5h under the conditions of 42 DEG C of temperature, mixture B are made；
(3) mixture B is placed on mixer, mixing 35min is carried out at 140 DEG C, after standing 12h, then be placed in mixing
On machine, carries out being kneaded 25min discharging at 170 DEG C, obtain rubber compound；
(4) above-mentioned rubber compound is placed on calender, with 100kg.cm-2Pressure, the pushing of 130 DEG C of temperature conditions prolongs into
Piece is to get nano combined absorbing material.
Speed of agitator in the preparation process is 300r/min.
Embodiment 4
A kind of nano combined absorbing material, is prepared by the raw material of following parts by weight: epoxy resin E-44 60 part, nanometer
20 parts of graphene, 18 parts of magnetic nanometer, 15 parts of nano-titanium dioxide, 16 parts of nano zine oxide, nanometer cobalt oxide 10 part, nanometer
12 parts of tungstic acid, 9 parts of gamma-aminopropyl-triethoxy-silane, 8 parts of toluene di-isocyanate(TDI), benzotriazole -1- carbothioic acid alkene
5 parts of propyl amides, 7 parts of butylene terephthalate, 5 parts of neopelex, 6 parts of polybutylene terephthalate (PBT),
7 parts of polyamide, 40 parts of isopropanol, 20 parts of acetone.
The epoxide number of the epoxy resin E-44 is 0.46mol/100g, dielectric constant 3.4.
A kind of preparation method of nano combined absorbing material of the present invention, preparation step are as follows:
(1) by nano-graphene, magnetic nanometer, nano-titanium dioxide, nano zine oxide, nanometer cobalt oxide, nanometer three
Tungsten oxide, gamma-aminopropyl-triethoxy-silane are added in agitator tank, and isopropanol is then added and is stirred 40min, in 50 DEG C
Temperature under the conditions of continue stir 2h, be made mixture A；
(2) epoxy resin E-44 is added in acetone soln and is dissolved, is then added under stirring conditions
To into mixture A made from step (1), after stirring 20min, sequentially add under stirring conditions toluene di-isocyanate(TDI),
Benzotriazole -1- carbothioic acid allyl amide, butylene terephthalate, neopelex, poly terephthalic acid
Butanediol ester and polyamide continue to stir 4h under the conditions of 50 DEG C of temperature, mixture B are made；
(3) mixture B is placed on mixer, mixing 50min is carried out at 160 DEG C, after standing 20h, then be placed in mixing
On machine, carries out being kneaded 40min discharging at 200 DEG C, obtain rubber compound；
(4) above-mentioned rubber compound is placed on calender, with 120kg.cm-2Pressure, the pushing of 150 DEG C of temperature conditions prolongs into
Piece is to get nano combined absorbing material.
Speed of agitator in the preparation process is 600r/min.
Comparative example 1
Comparative example 1 the difference from embodiment 1 is that, be not added with nano-titanium dioxide in comparative example 1.
Comparative example 2
Comparative example 2 the difference from embodiment 1 is that, be not added with nano tungsten trioxide in comparative example 2.
Performance test
The test specimens for being prepared into 3mm thickness to absorbing material prepared by above embodiments and comparative example carry out correlated performance survey
Examination, test result is as follows shown in table 1:
Table 1
By above-mentioned test result it is found that Wave suction composite material prepared by the present invention is under 3mm thickness, minimum reflectance is situated between
Between -17.2~-18.6dB, for effective Absorber Bandwidth (< -10dB) up to 6.5~8.3GHz, wave absorbing efficiency is high, and in low-frequency range
Absorbing property is also shown, absorbing property is good, therefore nano wave-absorbing material produced by the present invention has a good application prospect.
Claims (5)
1. a kind of nano combined absorbing material, which is characterized in that be prepared by the raw material of following parts by weight: epoxy resin E-
4440-60 parts, 12-20 parts of nano-graphene, 10-18 parts of magnetic nanometer, 8-15 parts of nano-titanium dioxide, nano zine oxide 7-
16 parts, 5-10 parts of nanometer cobalt oxide, 6-12 parts of nano tungsten trioxide, 4-9 parts of gamma-aminopropyl-triethoxy-silane, toluene two it is different
3-8 parts of cyanate, 2-5 parts of benzotriazole -1- carbothioic acid allyl amide, 3-7 parts of butylene terephthalate, dodecyl
1-5 parts of benzene sulfonic acid sodium salt, 2-6 parts of polybutylene terephthalate (PBT), 4-7 parts of polyamide, 20-40 parts of isopropanol, acetone 10-20
Part.
2. a kind of nano combined absorbing material according to claim 1, which is characterized in that by the raw material system of following parts by weight
It is standby and obtain: 50 parts of epoxy resin E-44,16 parts of nano-graphene, 14 parts of magnetic nanometer, 12 parts of nano-titanium dioxide, nano oxygen
Change 11 parts of zinc, 8 parts of nanometer cobalt oxide, 9 parts of nano tungsten trioxide, 7 parts of gamma-aminopropyl-triethoxy-silane, toluene diisocynate
6 parts of ester, 3.5 parts of benzotriazole -1- carbothioic acid allyl amide, 5 parts of butylene terephthalate, neopelex
3 parts, 4 parts of polybutylene terephthalate (PBT), 5.5 parts of polyamide, 30 parts of isopropanol, 15 parts of acetone.
3. a kind of nano combined absorbing material according to claim 1, which is characterized in that the ring of the epoxy resin E-44
Oxygen value is 0.42-0.46mol/100g, dielectric constant 3.0-3.4.
4. a kind of described in any item preparation methods of nano combined absorbing material of claim 1-3, which is characterized in that preparation step
It is rapid as follows:
(1) nano-graphene, magnetic nanometer, nano-titanium dioxide, nano zine oxide, nanometer cobalt oxide, nanometer three are aoxidized
Tungsten, gamma-aminopropyl-triethoxy-silane are added in agitator tank, and isopropanol is then added and is stirred 20-40min, in 35-50
DEG C temperature under the conditions of continue stir 1-2h, be made mixture A；
(2) epoxy resin E-44 is added in acetone soln and is dissolved, then added it under stirring conditions
In mixture A made from step (1), after stirring 10-20min, toluene di-isocyanate(TDI), benzene are sequentially added under stirring conditions
And triazole -1- carbothioic acid allyl amide, butylene terephthalate, neopelex, poly terephthalic acid fourth
Diol ester and polyamide continue to stir 2-4h under the conditions of 40-50 DEG C of temperature, mixture B are made；
(3) mixture B is placed on mixer, mixing 30-50min is carried out at 130-160 DEG C, after standing 10-20h, then set
In on mixer, carrying out mixing 20-40min discharging at 160-200 DEG C, rubber compound is obtained；
(4) above-mentioned rubber compound is placed on calender, with the pressure of 90-120kg.cm-2,120-150 DEG C of temperature condition pushing is prolonged
In flakes to get nano combined absorbing material.
5. a kind of preparation method of nano combined absorbing material according to claim 4, which is characterized in that described to prepare
Speed of agitator in journey is 200-600r/min.
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Citations (4)
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|---|---|---|---|---|
| CN103554844A (en) * | 2013-10-29 | 2014-02-05 | 广东生益科技股份有限公司 | Thermosetting resin composition and application thereof |
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| CN108794992A (en) * | 2018-07-03 | 2018-11-13 | 佛山市影腾科技有限公司 | A kind of optical sensor package material |
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2019
- 2019-02-21 CN CN201910128250.6A patent/CN109796729A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103554844A (en) * | 2013-10-29 | 2014-02-05 | 广东生益科技股份有限公司 | Thermosetting resin composition and application thereof |
| CN104774472A (en) * | 2015-04-10 | 2015-07-15 | 大连东信微波技术有限公司 | Ultra-wideband terahertz wave-absorbing material |
| CN106752695A (en) * | 2016-12-08 | 2017-05-31 | 辽宁法库陶瓷工程技术研究中心 | High IR emissivity radiating antiradar coatings for electronic device and preparation method thereof |
| CN108794992A (en) * | 2018-07-03 | 2018-11-13 | 佛山市影腾科技有限公司 | A kind of optical sensor package material |
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Application publication date: 20190524 |