CN104693690A - Polyaniline/epoxy resin wave-absorbing composite material and preparation method thereof - Google Patents
Polyaniline/epoxy resin wave-absorbing composite material and preparation method thereof Download PDFInfo
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- CN104693690A CN104693690A CN201310654881.4A CN201310654881A CN104693690A CN 104693690 A CN104693690 A CN 104693690A CN 201310654881 A CN201310654881 A CN 201310654881A CN 104693690 A CN104693690 A CN 104693690A
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Abstract
The invention relates to a polyaniline/epoxy resin composite material and a preparation method thereof, belonging to the field of an electromagnetic wave-absorbing material. The polyaniline/epoxy resin composite material is prepared from the following components by weight: 100 parts of epoxy resin, 100 parts of polyaniline, 5 to 30 parts of magnetic filler, 5 to 30 parts of metal-doped oxide and 10 to 40 parts of a curing agent. Compared with the prior art, the invention has the following advantages: in situ polymerization is utilized to prepare polyaniline and secondary doping of polyaniline is carried out, so polyaniline is allowed to achieve conductivity with a best wave-absorbing property, and overall wave-absorbing property of the composite material is improved; dielectric-loss type polyaniline composites with magnetic-loss type carbonyl iron, so the wave-absorbing material with good dielectric loss and magnetic loss is obtained, and high-frequency wave-absorbing performance of the material is increased.
Description
Technical field
The invention belongs to electromagnetic-wave absorbent field, relate to a kind of polyaniline/epoxy resin composite material and preparation method thereof.
Background technology
Along with the development of science and technology and the development of industrial civilization, the electromagnetic pollution that increasing electronic and electrical equipment and communication system produce has penetrated into each corner of life, has a strong impact on the physical and mental health of people.Therefore, how effectively to prevent and to eliminate electromagnetic radiation and interference, become an important topic of development in science and technology.
Electromagnetic-wave absorbent refers to the electromagnetic wave energy that can absorb and project its surface, and makes electromagnetic wave energy be converted into a kind of material of heat or other form energies by the dielectric loss of material.The shortcomings such as traditional absorbing material, to absorb by force tail major objective, has absorption band narrow, and density is large; Novel wave-absorbing material then requires " thin, gently, wide, strong ", in this context, has conducting polymer that conjugated pi is good for becomes people study hotspot as novel absorbing material.
Wherein, polyaniline (PAni) is a kind of common dielectric loss type conductive polymers, and have various structures, density is low, and synthesis is simple, the advantages such as environmental stability is good, but its suction ripple frequency band is narrow, and matching thickness is large; Iron carbonyl is a kind of magneticmetal, have excellent fade performance, but density is large to the hertzian wave in high-frequency range.Therefore the two can be combined, with transparent polymer epoxy resin for matrix, prepare epoxide resin wave-absorbing matrix material.The impedance matching that the combination of polyaniline and iron carbonyl can improve material absorbs to increase, and also can reach simultaneously and open up wide band object.
Summary of the invention
The object of the present invention is to provide a kind of polyaniline/epoxide resin wave-absorbing matrix material.
Another object of the present invention is to provide a kind of preparation method of above-mentioned polyaniline/epoxide resin wave-absorbing matrix material.
For achieving the above object, technical scheme of the present invention is as follows:
A kind of epoxy resin composite material, this matrix material is made up of the component comprising following weight part:
Described epoxy resin is bisphenol A type epoxy resin, is preferably E-54, E-44 or E-51.(E-54, E-44 or E-51 are the epoxy resin trade mark, are the rotten Technology Co., Ltd. of the blue coast defence of Qingdao Hua Chang and produce)
Described polyaniline is self-control, and microscopic pattern is particulate state, and particle diameter is 1 ~ 2 μm, is that (homemade polyaniline, can control polyaniline microscopic pattern to black powder, i.e. particulate state after grinding.）。
Described solidifying agent is 4,4 '-diaminodiphenyl-methane (DDM), quadrol, diaminodiphenylmethane, Dicyanodiamide or diamino diphenyl sulfone.
Described magnetic fillers is carbonyl iron particles, black powder, and microscopic pattern is spheroidal particle, particle diameter 2 ~ 3 μm.
Described metal-doped oxide compound is for mixing manganese zinc oxide, and wherein zinc oxide microscopic pattern is three-dimensional four needle-like three-dimensional arrangements, and particle diameter is 2 ~ 5 μm.
Described magnetic fillers is identical with metal-doped oxide compound consumption.
A preparation method for above-mentioned epoxy resin composite material, the method includes the steps of:
(1) polyaniline is prepared;
(2) preparation of polyaniline/epoxy resin composite material: 100 parts of obtained for step (1) polyanilines, 5 ~ 30 parts of magneticsubstances, 5 ~ 30 parts of metal-doped oxide compounds are added 100 parts of epoxy resin, and mechanical stirring under room temperature, mixes; Then add 10 ~ 40 parts of solidifying agent, pour in mould after ultrasonic 5 ~ 15min further, at 60 ~ 80 DEG C after solidification, remove mould, namely obtain epoxy resin composite material.
In described step (1), the preparation of polyaniline comprises the following steps:
(1a) 100mol ammonium persulphate is dissolved in 0.05 ~ 0.2mol/L hydrochloric acid soln of 200L, slowly drip aniline monomer in the solution, at-5 ~ 5 DEG C, react 12 ~ 24h, it is clean that reaction terminates rear deionized water wash, and at 60 ~ 80 DEG C, vacuum-drying obtains polyaniline;
(1b) be dissolved in the hydrochloric acid soln of 1mol/L by polyaniline obtained for step (1a) and carry out secondary doping, stirred overnight, after standing separation, vacuum-drying at 60 ~ 80 DEG C, with stand-by after ball mill abrasive dust.
In described step (1a), the rate of addition of aniline monomer is 3 ~ 5 seconds/.
In described step (1a), the mol ratio of aniline monomer and ammonium persulphate is 1.1:1.
The present invention compared with the existing technology, has the following advantages:
(1) the present invention utilizes in-situ polymerization to prepare polyaniline, and carries out secondary doping to it, polyaniline is reached have the specific conductivity of best absorbing property, improves the absorbing property of composites;
(2) iron carbonyl of the polyaniline of dielectric loss type and magnetic loss type is carried out compound by the present invention, obtains the absorbing material with good dielectric loss and magnetic losses, increases the high frequency absorbing property of material;
(3) the present invention will be used for metal-doped oxide compound and the magnetic fillers of infrared absorption, conductive filler material compound, effectively can increase the low frequency absorbing property of matrix material, widen the suction ripple frequency band of matrix material;
(4) filler powder is dispersed in transparent epoxy resin by the present invention, has easy-formation, easy to process, is suitable for the features such as a large amount of productions, and gained matrix material is to stronger to absorption of electromagnetic wave power, and quality is lighter.
Embodiment
The present invention is further illustrated below in conjunction with embodiment.
In the following example:
The HP8722ES type vector network analyzer that the polyaniline prepared/epoxide resin wave-absorbing matrix material is produced by using Agilent company, under frequency 8-18GHz, carries out the test of absorbing property to the matrix material obtained in following case study on implementation;
The 8510B type vector network analyzer that the polyaniline prepared/epoxide resin wave-absorbing matrix material is produced by using Agilent company, under frequency 0.5GHz-2GHz, carries out microwave reflection loss test to the matrix material obtained in following case study on implementation;
Embodiment 1
(1) preparation of polyaniline:
100mol ammonium persulphate is dissolved in the 0.05mol/L hydrochloric acid soln of 200L, slowly keep in the solution dripping an aniline monomer Ai in 3 ~ 5 seconds, (wherein the mol ratio of aniline monomer and ammonium persulfate is 1.1:1), 12h is reacted at-5 DEG C, it is clean that reaction terminates rear deionized water wash, vacuum-drying at 60 DEG C; Be dissolved in the hydrochloric acid soln of 1mol/L by the above-mentioned polyaniline preparing gained and carry out secondary doping, stirred overnight, after standing separation, vacuum-drying at 60 DEG C, with stand-by after ball mill abrasive dust;
(2) preparation of polyaniline/epoxide resin wave-absorbing matrix material:
By 100 parts of polyanilines, 5 parts of carbonyl iron dusts, lead Al-Doped ZnO for 5 parts to add respectively in 100 parts of epoxy resin, mechanical stirring under room temperature, after mixing, add 10 parts of Dicyanodiamides, pour in mould after ultrasonic 5 ~ 15min further, at 60 ~ 80 DEG C after solidification, remove mould, coat-thickness is 3mm, namely obtains epoxy resin composite material of the present invention.
Embodiment 2
(1) preparation of polyaniline:
100mol ammonium persulphate is dissolved in the 0.08mol/L hydrochloric acid soln of 200L, slowly drip aniline monomer Ai in the solution, (wherein the mol ratio of aniline monomer and ammonium persulfate is 1.1:1), reacts 14h at-3 DEG C, it is clean that reaction terminates rear deionized water wash, vacuum-drying at 65 DEG C; Be dissolved in the hydrochloric acid soln of 1mol/L by the above-mentioned polyaniline preparing gained and carry out secondary doping, stirred overnight, after standing separation, vacuum-drying at 65 DEG C, with stand-by after ball mill abrasive dust;
(2) preparation of polyaniline/epoxide resin wave-absorbing matrix material:
By 100 parts of polyanilines, 8 parts of carbonyl iron dusts, mix aluminum oxidation for 8 parts and add epoxy resin by a certain percentage, mechanical stirring under room temperature, after mixing, add 15 parts of quadrols, pour in mould after ultrasonic 5 ~ 15min further, at 60 ~ 80 DEG C after solidification, remove mould, coat-thickness is 3mm, namely obtains epoxy resin composite material of the present invention.
Embodiment 3
(1) preparation of polyaniline:
100mol ammonium persulphate is dissolved in the 0.1mol/L hydrochloric acid soln of 200L, slowly drip aniline monomer Ai in the solution, (wherein the mol ratio of aniline monomer and ammonium persulfate is 1.1:1), reacts 16h at-1 DEG C, it is clean that reaction terminates rear deionized water wash, vacuum-drying at 70 DEG C; Be dissolved in the hydrochloric acid soln of 1mol/L by the above-mentioned polyaniline preparing gained and carry out secondary doping, stirred overnight, after standing separation, vacuum-drying at 70 DEG C, with stand-by after ball mill abrasive dust;
(2) preparation of polyaniline/epoxide resin wave-absorbing matrix material:
By 100 parts of polyanilines, 11 parts of carbonyl iron dusts, 11 parts of Al-Doped ZnOs add epoxy resin by a certain percentage, and mechanical stirring under room temperature, after mixing, add 20 parts of quadrols, pour in mould after ultrasonic 5 ~ 15min further, at 60 ~ 80 DEG C after solidification, remove mould, coat-thickness is 3mm, namely obtains epoxy resin composite material of the present invention.
Embodiment 4
(1) preparation of polyaniline:
100mol ammonium persulphate is dissolved in the 0.15mol/L hydrochloric acid soln of 200L, slowly drip aniline monomer Ai in the solution, (wherein the mol ratio of aniline monomer and ammonium persulfate is 1.1:1), reacts 18h at 0 DEG C, it is clean that reaction terminates rear deionized water wash, vacuum-drying at 75 DEG C; Be dissolved in the hydrochloric acid soln of 1mol/L by the above-mentioned polyaniline preparing gained and carry out secondary doping, stirred overnight, after standing separation, vacuum-drying at 75 DEG C, with stand-by after ball mill abrasive dust;
(2) preparation of polyaniline/epoxide resin wave-absorbing matrix material:
By 100 parts of polyanilines, 14 parts of carbonyl iron dusts, 14 parts of Al-Doped ZnOs add epoxy resin by a certain percentage, mechanical stirring under room temperature, after mixing, add 25 part 4,4 '-diaminodiphenyl-methane, pour in mould after ultrasonic 5 ~ 15min further, at 60 ~ 80 DEG C after solidification, remove mould, coat-thickness is 3mm, namely obtains epoxy resin composite material of the present invention.
Embodiment 5
(1) preparation of polyaniline:
100mol ammonium persulphate is dissolved in the 0.18mol/L hydrochloric acid soln of 200L, slowly drip aniline monomer Ai in the solution, (wherein the mol ratio of aniline monomer and ammonium persulfate is 1.1:1), reacts 20h at 1 DEG C, it is clean that reaction terminates rear deionized water wash, vacuum-drying at 80 DEG C; Be dissolved in the hydrochloric acid soln of 1mol/L by the above-mentioned polyaniline preparing gained and carry out secondary doping, stirred overnight, after standing separation, vacuum-drying at 80 DEG C, with stand-by after ball mill abrasive dust;
(2) preparation of polyaniline/epoxide resin wave-absorbing matrix material:
By 100 parts of polyanilines, 17 parts of carbonyl iron dusts, 17 parts of Al-Doped ZnOs add epoxy resin by a certain percentage, and mechanical stirring under room temperature, after mixing, add 30 parts of diaminodiphenylmethane, pour in mould after ultrasonic 5 ~ 15min further, at 60 ~ 80 DEG C after solidification, remove mould, coat-thickness is 3mm, namely obtains epoxy resin composite material of the present invention.
Embodiment 6
(1) preparation of polyaniline:
100mol ammonium persulphate is dissolved in the 0.2mol/L hydrochloric acid soln of 200L, slowly drip aniline monomer Ai in the solution, (wherein the mol ratio of aniline monomer and ammonium persulfate is 1.1:1), reacts 22h at 3 DEG C, it is clean that reaction terminates rear deionized water wash, vacuum-drying at 60 DEG C; Be dissolved in the hydrochloric acid soln of 1mol/L by the above-mentioned polyaniline preparing gained and carry out secondary doping, stirred overnight, after standing separation, vacuum-drying at 60 DEG C, with stand-by after ball mill abrasive dust;
(2) preparation of polyaniline/epoxide resin wave-absorbing matrix material:
By 100 parts of polyanilines, 20 parts of carbonyl iron dusts, 20 parts of Al-Doped ZnOs add epoxy resin by a certain percentage, mechanical stirring under room temperature, after mixing, add 30 part 4,4 '-diaminodiphenyl-methane, pour in mould after ultrasonic 5 ~ 15min further, at 60 ~ 80 DEG C after solidification, remove mould, coat-thickness is 3mm, namely obtains epoxy resin composite material of the present invention.
Embodiment 7
(1) preparation of polyaniline:
100mol ammonium persulphate is dissolved in the 0.1mol/L hydrochloric acid soln of 200L, slowly drip aniline monomer Ai in the solution, (wherein the mol ratio of aniline monomer and ammonium persulfate is 1.1:1), reacts 24h at 0 DEG C, it is clean that reaction terminates rear deionized water wash, vacuum-drying at 70 DEG C; Be dissolved in the hydrochloric acid soln of 1mol/L by the above-mentioned polyaniline preparing gained and carry out secondary doping, stirred overnight, after standing separation, vacuum-drying at 70 DEG C, with stand-by after ball mill abrasive dust;
(2) preparation of polyaniline/epoxide resin wave-absorbing matrix material:
By 100 parts of polyanilines, 25 parts of carbonyl iron dusts, 25 parts of Al-Doped ZnOs add epoxy resin by a certain percentage, and mechanical stirring under room temperature, after mixing, add 35 parts of diamino diphenyl sulfones, pour in mould after ultrasonic 5 ~ 15min further, at 60 ~ 80 DEG C after solidification, remove mould, coat-thickness is 3mm, namely obtains epoxy resin composite material of the present invention.
Embodiment 8
(1) preparation of polyaniline:
100mol ammonium persulphate is dissolved in the 0.1mol/L hydrochloric acid soln of 200L, slowly drip aniline monomer Ai in the solution, (wherein the mol ratio of aniline monomer and ammonium persulfate is 1.1:1), reacts 24h at 5 DEG C, it is clean that reaction terminates rear deionized water wash, vacuum-drying at 60 DEG C; Be dissolved in the hydrochloric acid soln of 1mol/L by the above-mentioned polyaniline preparing gained and carry out secondary doping, stirred overnight, after standing separation, vacuum-drying at 60 DEG C, with stand-by after ball mill abrasive dust;
(2) preparation of polyaniline/epoxide resin wave-absorbing matrix material:
By 100 parts of polyanilines, 30 parts of carbonyl iron dusts, 30 parts of Al-Doped ZnOs add epoxy resin by a certain percentage, and mechanical stirring under room temperature, after mixing, add 40 parts of diamino diphenyl sulfones, pour in mould after ultrasonic 5 ~ 15min further, at 60 ~ 80 DEG C after solidification, remove mould, coat-thickness is 3mm, namely obtains epoxy resin composite material of the present invention.
Table 1
The epoxy resin composite wave-absorbing material prepared by example 1 ~ 8 goes to test in 0.5GHz-2GHz low frequency range and 8-18GHz high frequency respectively, can find to draw a conclusion: (1) metal mixes and effectively increases the absorbing property of matrix material at low frequency place adding of oxide compound, and matrix material maximum reflectivity in 0.5GHz-2GHz range of frequency can reach 14.5dB; (2) along with the increase of magnetic-particle iron carbonyl content, the peak value of matrix material in 8GHz-18GHz range of frequency is progressively to high-frequency mobile, the maximum reflectivity being 16.13GHz place in frequency can reach 28.6dB, therefore, iron carbonyl add the magnetic property that effectively can improve composite wave-suction material, make material have excellent absorbing property at high frequency treatment simultaneously; In sum, will metal-doped oxide compound and the magnetic fillers of infrared absorption, conductive filler material compound be used for, effectively can increase the absorbing property of matrix material, widen the suction ripple frequency band of matrix material.
Above-mentioned is can understand and apply the invention for ease of those skilled in the art to the description of embodiment.Person skilled in the art obviously easily can make various amendment to these embodiments, and General Principle described herein is applied in other embodiments and need not through performing creative labour.Therefore, the invention is not restricted to embodiment here, those skilled in the art, according to announcement of the present invention, do not depart from improvement that scope makes and amendment all should within protection scope of the present invention.
Claims (10)
1. an epoxy resin composite material, is characterized in that: this matrix material is made up of the component comprising following weight part:
2. epoxy resin composite material according to claim 1, is characterized in that: described epoxy resin is bisphenol A type epoxy resin, is preferably E-54, E-44 or E-51.
3. epoxy resin composite material according to claim 1, is characterized in that: described polyaniline to be particle diameter the be particle of 1 ~ 2 μm.
4. epoxy resin composite material according to claim 1, is characterized in that: described solidifying agent is 4,4 '-diaminodiphenyl-methane, quadrol, diaminodiphenylmethane, Dicyanodiamide or diamino diphenyl sulfone.
5. epoxy resin composite material according to claim 1, is characterized in that: described magnetic fillers is carbonyl iron particles, and particle diameter is 2 ~ 3 μm.
6. epoxy resin composite material according to claim 1, is characterized in that: described metal-doped oxide compound is for mixing manganese zinc oxide, and wherein zinc oxide microscopic pattern is three-dimensional four needle-like three-dimensional arrangements, and particle diameter is 2 ~ 5 μm.
7. epoxy resin composite material according to claim 1, is characterized in that: described magnetic fillers is identical with metal-doped oxide compound consumption.
8. the preparation method of arbitrary described epoxy resin composite material in claim 1-7, is characterized in that: the method includes the steps of:
(1) polyaniline is prepared;
(2) polyaniline/epoxy resin composite material is prepared: 100 parts of obtained for step (1) polyanilines, 5 ~ 30 parts of magneticsubstances, 5 ~ 30 parts of metal-doped oxide compounds are added 100 parts of epoxy resin, and mechanical stirring under room temperature, mixes; Then add 10 ~ 40 parts of solidifying agent, pour in mould after ultrasonic 5 ~ 15min further, at 60 ~ 80 DEG C after solidification, remove mould, namely obtain epoxy resin composite material.
9. preparation method according to claim 8, is characterized in that: in described step (1), the preparation of polyaniline comprises the following steps:
(1a) 100mol ammonium persulphate is dissolved in 0.05 ~ 0.2mol/L hydrochloric acid soln of 200L, slowly drip aniline monomer in the solution, at-5 ~ 5 DEG C, react 12 ~ 24h, it is clean that reaction terminates rear deionized water wash, and at 60 ~ 80 DEG C, vacuum-drying obtains polyaniline;
(1b) be dissolved in the hydrochloric acid soln of 1mol/L by polyaniline obtained for step (1a) and carry out secondary doping, stirred overnight, after standing separation, vacuum-drying at 60 ~ 80 DEG C, with stand-by after ball mill abrasive dust.
10. preparation method according to claim 9, is characterized in that: in described step (1a), the rate of addition of aniline monomer is 3 ~ 5 seconds/;
Or in described step (1a), the mol ratio of aniline monomer and ammonium persulphate is 1.1:1.
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| CN115926455A (en) * | 2023-01-17 | 2023-04-07 | 河南城建学院 | Epoxy resin reinforced zinc stannate @ polyaniline aerogel composite sound absorption material and preparation method thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105199383A (en) * | 2015-10-27 | 2015-12-30 | 苏州宽温电子科技有限公司 | Polyaniline magnetic composite material and preparation method thereof |
| CN106433120A (en) * | 2016-08-17 | 2017-02-22 | 北京君研碳极科技有限公司 | Preparation method for composite anti-electromagnetic wave radiation material of polyaniline/coal-to-oil residues and product prepared by same |
| CN112143341A (en) * | 2020-10-14 | 2020-12-29 | 湖南科技大学 | Preparation method of secondary POSS-doped modified polyaniline anticorrosive coating |
| CN112143341B (en) * | 2020-10-14 | 2022-04-01 | 湖南科技大学 | Preparation method of secondary POSS-doped modified polyaniline anticorrosive coating |
| CN115926455A (en) * | 2023-01-17 | 2023-04-07 | 河南城建学院 | Epoxy resin reinforced zinc stannate @ polyaniline aerogel composite sound absorption material and preparation method thereof |
| CN115926455B (en) * | 2023-01-17 | 2024-03-29 | 河南城建学院 | Epoxy resin reinforced zinc stannate@polyaniline aerogel composite sound absorption material and preparation method thereof |
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Denomination of invention: Polyaniline/epoxy resin wave-absorbing composite material and preparation method thereof Effective date of registration: 20191202 Granted publication date: 20180918 Pledgee: Chuzhou economic and Technological Development Corporation Pledgor: Shanghai Jieshijie New Materials (Group) Co., Ltd. Registration number: Y2019980000815 |