CN1696212A - Ferrous powder absorbent, preparation method and application - Google Patents
Ferrous powder absorbent, preparation method and application Download PDFInfo
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- CN1696212A CN1696212A CN 200410037833 CN200410037833A CN1696212A CN 1696212 A CN1696212 A CN 1696212A CN 200410037833 CN200410037833 CN 200410037833 CN 200410037833 A CN200410037833 A CN 200410037833A CN 1696212 A CN1696212 A CN 1696212A
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Abstract
An iron powder absorbent for preparing the electromagnet wave absorbing-shielding material is prepared from iron powder through modifying the surface of iron particles by coupling agent and solvent.
Description
Technical field
The present invention relates to a kind of iron powder absorption agent that is used for absorption of electromagnetic wave and shielding material and its production and application, specifically, the present invention relates to iron powder absorption agent of a kind of surface modification that is used for absorption of electromagnetic wave and shielding material and its production and application.
Background technology
Along with the development of information technology, the infosystem that people used and relied on is more and more, and these infosystems are all transmitted by means of digitized signal, produces error so be easy to be subjected to Electromagnetic Interference (EMI).Have been found that from the Electromagnetic Interference of electronics and information equipment to cause tangible fault, for example the medical facilities of hospital and user's electronics.Especially, various sophisticated weapons, military communication command system have all used high electronics of a large amount of sensitivity and instrument in modern war, very responsive to Electromagnetic Interference, because the matters of aggravation that Electromagnetic Interference causes occurs repeatedly, therefore this just the reliability requirement to electronic devices and components in the complete machine and detection part is more and more higher, prevent that particularly electronic pollution, electromagenetic wave radiation and interferential index are also more and more higher.The hertzian wave of electronics radiation in addition,, leakage is also threatening human beings'health and safety.The harm that how Electromagnetic Interference is caused is reduced to minimum degree, all has great importance aspect the HUMAN HEALTH in national defence, civilian and even protection.Though prevent that the technology kind of Electromagnetic Interference is a lot, more generally the method for Cai Yonging is to use electromagnetic wave absorbent material and electromagnetic shielding material.Electromagnetic wave absorbent material and electromagnetic shielding material normally are made up of polymer organic matrixs such as inorganic absorbent and plastics, rubber, tackiness agent, coating, absorption agent provides absorption of electromagnetic wave and the needed electromagnetic performance of shielding material, and macromolecule matrix is the carrier of absorption agent.The superfine iron powder absorption agent is owing to the Curie temperature height, and temperature stability is good; In magneticsubstance, have the highest specific saturation magnetization at present, microwave magnetic permeability is bigger; Specific inductivity is bigger, thereby has obtained widespread use in absorption of electromagnetic wave and shielding material field.Because macromolecular material has hydrophobicity, inorganic absorbent iron powder possess hydrophilic property, if handle without modification on the iron powder surface, after it is added in the polymer organic matrix, cause between iron powder and the matrix interfacial combined function bad because both interface is incompatible, the absorption of electromagnetic wave and the use properties of shielding material of deterioration preparation are as mechanical property, aging resistance decline, cause inorganic absorbent iron powder loading level not high simultaneously, thus poor to absorption of electromagnetic wave and shield effectiveness.Therefore, the inorganic absorbent iron powder must carry out surface modification through physics or chemical treatment as the filled media of microwave absorbing and shielding material.But do not see have the iron powder of large usage quantity in absorption of electromagnetic wave and shielding material absorption agent that it is carried out the report of surface modification at present.
Summary of the invention
The present invention has proposed iron powder absorption agent of a kind of surface modification and its production and application in order to solve problem such as iron powder and the organic substance bonding properties is poor, loading level is low, poor mechanical property in the prior art.
Specific embodiments of the present invention is as follows:
Iron powder absorption agent of the present invention is made up of the component of following weight per-cent: iron powder 90.91～99.95%, coupling agent 0.05～9.09%, solvent 0～0.5%.
At least a in the preferred reduced iron powder of described iron powder, the carbonyl iron dust, particle shape is sphere or almost spherical, and the weight percent content of ferro element is greater than 95%, and median size is 0.1～50 μ m.
The mixture of one or more in described coupling agent preferred silane coupling agent, titanate coupling agent, zirconium ester coupling agent, the aluminate coupling agent.
The mixture of one or more in the preferred distilled water oil of described solvent, sherwood oil, methylethylketone, acetone, methyl alcohol, ethanol, ethylene glycol, Virahol, n-propyl alcohol, benzene, the second benzene,toluene,xylene.
Iron powder described in the present invention, coupling agent and solvent are the commercially available prod.
The preparation method of iron powder absorption agent of the present invention may further comprise the steps:
(1) under 0～50 ℃ temperature, coupling agent and solvent are stirred with agitator, or even with ultrasonic dispersing, make surface-modifying agent;
(2) iron powder that needs is carried out surface modification joins in the surface-modifying agent that step (1) obtains, and dries in Vacuumdrier then, obtains iron powder absorption agent of the present invention.
The consumption of the coupling agent described in the step (1) be preferably pre-modification iron powder weight 0.05～10%, the consumption of described solvent be preferably pre-modification iron powder weight 10～100%.
Have no particular limits stirring in described step (1), can use common agitator to stir, stirring velocity is 20～1400 rev/mins, and the time of stirring is to get final product in 20～50 minutes; Also can use ultrasonic wave to mix 5～25 minutes to evenly getting final product, ultrasonic frequency is 20KHz～50KHz, and power is 50W～5000W.
Oven dry described in the step (2) is preferably: vacuum tightness is-0.05～-0.1Mpa, bake out temperature is 30～90 ℃, be 6～18h time of drying.The solvent major part that the oven dry of this step of process adds vapors away, a little residue part, and therefore the solvent in the iron powder absorption agent of the present invention only is residual volume or does not have.
Iron powder absorption agent of the present invention is applied in absorption of electromagnetic wave and the shielding material.Specifically it can be applied in plastics, rubber, tackiness agent, coating etc. in the absorption of electromagnetic wave of matrix and the shielding material.Using method is an ordinary method.
The present invention has carried out surface modification to iron powder, and operation is simple and feasible for method, is easy to realize suitability for industrialized production.Because exist the functional group of two kinds of character in the coupling agent molecule structure, the polar group on a kind of functional group and inorganic absorbent iron powder surface reacts, another functional group can react with organism.Iron powder after the modification is compared with the iron powder of not modification, very big variation has taken place in its surface properties, change hydrophobicity into by wetting ability, lipophilicity, processing characteristics increase greatly, after joining in the organic substance matrix as the absorption agent filler, improve the bonding properties of iron powder absorption agent and organic matrix, can obviously improve the mechanical property that polymer-based hertzian wave is inhaled ripple, shielding material, improved the loading level of iron powder in macromolecule matrix.
Description of drawings
Fig. 1 adds the not latter made section surface sweeping of the iron powder electromicroscopic photograph of surface modification in the rubber of application example;
Fig. 2 adds the latter made section surface sweeping of the iron powder electromicroscopic photograph of surface modification of the present invention for the rubber of application example.
Embodiment
Adopt the mode of embodiment to further specify iron powder absorption agent of surface modification of the present invention and preparation method thereof below, but the present invention is not limited to these embodiment.
Example 1
Take by weighing silane coupling agent gamma-chloropropylmethyldimethoxysilane 2kg, dehydrated alcohol 60kg joins in the container, mixes making surface-modifying agent in 15 minutes under 25 ℃ in Ultrasonic Cleaners with ultrasonic wave; Take by weighing the reduced iron powder that the 100kg median size is 1.8 μ, pour in the container that surface-modifying agent is housed; Send into Vacuumdrier then, 60 ℃, oven dry 8h, vacuum tightness is-0.1MPa; Obtain the iron powder absorption agent of surface modification after the oven dry.
Example 2
Take by weighing titanate coupling agent sec.-propyl three (dioctyl is phosphate-based) titanic acid ester (NanJing Shuguang Chemical Group Co., Ltd.'s product) 2kg, acetone 50kg joins in the container, and 40 ℃ of following stirrings were made surface-modifying agent, 800 rev/mins of stirring velocitys in 20 minutes; Take by weighing the carbonyl iron dust that the 100kg median size is 5.0 μ, pour in the container that surface-modifying agent is housed; Send into Vacuumdrier then, 70 ℃, oven dry 10h, vacuum tightness is-0.08MPa; Obtain the iron powder absorption agent of surface modification after the oven dry.
Example 3
Take by weighing zirconium ester coupling agent TYZOR NBZ alkyl zirconate (E.I.Du Pont Company's product) 2kg, Virahol 40kg joins in the container, mixes making surface-modifying agent in 8 minutes under 30 ℃ in Ultrasonic Cleaners with ultrasonic wave; Take by weighing the carbonyl iron dust that the 100kg median size is 6.0 μ, pour in the container that surface-modifying agent is housed; Send into Vacuumdrier then, 80 ℃, oven dry 12h, vacuum tightness is-0.1MPa; Obtain the iron powder absorption agent of surface modification after the oven dry.
Example 4
Take by weighing aluminate coupling agent DL-411-B type (Fujian Normal University's demonstration plant's product) 2kg, dimethylbenzene 80kg joins in the container, and 40 ℃ of following stirrings were made surface-modifying agent, 700 rev/mins of stirring velocitys in 20 minutes; Take by weighing the carbonyl iron dust that the 100kg median size is 25.0 μ, pour in the container that surface-modifying agent is housed; Send into Vacuumdrier then, 60 ℃, oven dry 16h, vacuum tightness is-0.05MPa; Obtain the iron powder absorption agent of surface modification after the oven dry.
Application example
This example is the Application Example of iron powder absorption agent of the present invention, so that effect of the present invention to be described.
It is in the electromagnetic wave absorbent material of matrix that iron powder after the modification is joined with ethylene-propylene rubber(EPR) as the absorption agent filler, can obviously improve the mechanical property of this electromagnetic wave absorbent material.Concrete preparation process is as follows:
(1) takes by weighing silane coupling agent aminopropyl triethoxysilane that accounts for iron powder weight 0.5～2% and the ethanol that accounts for iron powder weight 15～50% respectively, be prepared into surface-modifying agent in 15 minutes with the ultrasonic wave mixing under 30 ℃, use preparation method of the present invention to prepare iron powder 603～612g (iron powder 600g wherein of surface modification, coupling agent 3～12g, ethanol＜1.0g); Take by weighing surperficial unmodified iron powder 600g in addition;
(2) take by weighing 100g ethylene-propylene rubber(EPR) respectively, each two parts of 3～8g vulcanizing agents, modification iron powder and unmodified iron powder and rubber and vulcanizing agent are carried out on twin-roll plastic mixing mill respectively mixing, slice;
(3) above-mentioned sizing material is respectively taken by weighing certainweight, under the same conditions sulfuration (140～180 ℃ of temperature, pressure 8～20MPa, curing time 10～40 minutes);
(4) measure mechanical property by national standard, measuring result such as following table:
| Tensile strength sigma/(MPa) | Tensile yield ε/(%) | Tension set Hd/ (%) | Tear strength ψ s/ (kN/m) | Shao Er A type hardness tester/degree | |
| The suction ripple shielding material that adds unmodified iron powder | ??4.43 | ??264 | ??7.5 | ??17.64 | ??80 |
| The suction ripple shielding material that adds the modification iron powder | ??10.20 | ??117 | ??0.9 | ??21.0 | ??85 |
As can be seen from the above table, the mechanical property of the electromagnetic wave absorbent material of adding modification iron powder is obviously good than the material that adds unmodified iron powder.
Section to two kinds of materials is made stereoscan photograph Fig. 1 and Fig. 2.See having tangible powder to extract effect on the microwave absorbing material section that does not have treated iron powder to fill from the section surface sweeping electromicroscopic photograph of the electromagnetic wave absorbent material made, fracture occurs in the bonding surface of powder and glue, and the interface is in conjunction with bad; Through the microwave absorbing material that the iron powder of this art breading is filled, section is neat, and fracture occurs in rubber matrix, and iron powder and rubber matrix consistency are fine, in conjunction with tight.
Claims (10)
1. an iron powder absorption agent is characterized in that, it is made up of the component of following weight per-cent: iron powder 90.91～99.95%, coupling agent 0.05～9.09%, solvent 0～0.5%.
2. iron powder absorption agent according to claim 1, it is characterized in that described iron powder is at least a in reduced iron powder, the carbonyl iron dust, particle shape is sphere or almost spherical, the weight percent content of ferro element is greater than 95%, and median size is 0.1～50 μ m.
3. iron powder absorption agent according to claim 1 is characterized in that, described coupling agent is one or more the mixture in silane coupling agent, titanate coupling agent, zirconium ester coupling agent, the aluminate coupling agent.
4. iron powder absorption agent according to claim 1, it is characterized in that described solvent is one or more the mixture in distilled water oil, sherwood oil, methylethylketone, acetone, methyl alcohol, ethanol, ethylene glycol, Virahol, n-propyl alcohol, benzene, the second benzene,toluene,xylene.
5. iron powder absorption agent according to claim 1 is characterized in that it is prepared by following preparation method:
(1) under 0～50 ℃ temperature, coupling agent and solvent are stirred with agitator, or even with ultrasonic dispersing, make surface-modifying agent;
(2) iron powder that needs is carried out surface modification joins in the surface-modifying agent that step (1) obtains, and dries in Vacuumdrier then, obtains iron powder absorption agent of the present invention.
6. the preparation method of the described iron powder absorption agent of claim 1 is characterized in that, may further comprise the steps:
(1) under 0～50 ℃ temperature, coupling agent and solvent are stirred with agitator, or even with ultrasonic dispersing, make surface-modifying agent;
(2) iron powder that needs is carried out surface modification joins in the surface-modifying agent that step (1) obtains, and dries in Vacuumdrier then, obtains iron powder absorption agent of the present invention.
7. preparation method according to claim 6 is characterized in that, the consumption of the coupling agent described in the step (1) be pre-modification iron powder weight 0.05～10%, the consumption of described solvent be pre-modification iron powder weight 10～100%.
8. preparation method according to claim 6 is characterized in that, the time of stirring with agitator in the step (1) is 20～50 minutes, and stirring velocity is 20～1400 rev/mins; Time with ultrasonic dispersing is 5～25 minutes, and ultrasonic frequency is 20KHz～50KHz, and power is 50W～5000W.
9. preparation method according to claim 6 is characterized in that, described oven dry is: vacuum tightness is-0.05～-0.1Mpa, bake out temperature is 30～90 ℃, be 6～18h time of drying.
10. the application of the described iron powder absorption agent of claim 1 in absorption of electromagnetic wave and shielding material.
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| Application Number | Priority Date | Filing Date | Title |
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| CNB2004100378331A CN100351322C (en) | 2004-05-11 | 2004-05-11 | Ferrous powder absorbent, preparation method and application |
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| CNB2004100378331A CN100351322C (en) | 2004-05-11 | 2004-05-11 | Ferrous powder absorbent, preparation method and application |
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| CN1696212A true CN1696212A (en) | 2005-11-16 |
| CN100351322C CN100351322C (en) | 2007-11-28 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100429023C (en) * | 2006-09-20 | 2008-10-29 | 电子科技大学 | Magnetic micro powder and method for making same |
| CN105290421A (en) * | 2015-11-11 | 2016-02-03 | 芜湖迈科威特新材料有限公司 | Preparation method of S-waveband wave absorbing material |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| DE3602373A1 (en) * | 1985-01-31 | 1986-08-07 | Mitsubishi Petrochemical Co., Ltd., Tokio/Tokyo | METAL POWDER CONTAINING POLYMER COMPOSITION |
| JPH01256567A (en) * | 1988-04-05 | 1989-10-13 | Showa Denko Kk | Resin composition |
| JP3009695B2 (en) * | 1990-01-26 | 2000-02-14 | 戸田工業株式会社 | Iron-based magnetic particle powder and method for producing the same |
| JPH0480274A (en) * | 1990-07-23 | 1992-03-13 | Tokin Corp | Electric radiation absorber composition |
| CN1320602A (en) * | 2001-01-16 | 2001-11-07 | 天津大学 | Retinyl Schiff's base-iron complex as microwave absorbent and its preparing process |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100429023C (en) * | 2006-09-20 | 2008-10-29 | 电子科技大学 | Magnetic micro powder and method for making same |
| CN105290421A (en) * | 2015-11-11 | 2016-02-03 | 芜湖迈科威特新材料有限公司 | Preparation method of S-waveband wave absorbing material |
| CN105290421B (en) * | 2015-11-11 | 2018-04-03 | 芜湖迈科威特新材料有限公司 | A kind of preparation method of S-band absorbing material |
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| CN100351322C (en) | 2007-11-28 |
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Assignee: Jiangsu Huaxing Electronic Co., Ltd. Assignor: Nanjing University of Technology Contract fulfillment period: 2007.12.5 to 2015.12.4 contract change Contract record no.: 2008320000379 Denomination of invention: Ferrous powder absorbent, preparation method and application Granted publication date: 20071128 License type: Exclusive license Record date: 2008.9.25 |
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Free format text: EXCLUSIVE LICENCE; TIME LIMIT OF IMPLEMENTING CONTACT: 2007.12.5 TO 2015.12.4 Name of requester: JIANGSU HUAXING ELECTRON CO., LTD. Effective date: 20080925 |
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Granted publication date: 20071128 |