CN109867829A - A kind of carbonyl iron dust wave absorbing agent and preparation method thereof - Google Patents
A kind of carbonyl iron dust wave absorbing agent and preparation method thereof Download PDFInfo
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- CN109867829A CN109867829A CN201711262016.XA CN201711262016A CN109867829A CN 109867829 A CN109867829 A CN 109867829A CN 201711262016 A CN201711262016 A CN 201711262016A CN 109867829 A CN109867829 A CN 109867829A
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- carbonyl iron
- iron dust
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Abstract
The present invention provides a kind of carbonyl iron dust wave absorbing agents and preparation method thereof, method includes the following steps: carbonyl iron dust is added in organic solvent, add dispersion solvent, and dispersion obtains carbonyl iron dust dispersion liquid；Formaldehyde and melamine are mixed, mixed liquor is obtained, adjusts pH of mixed, insulation reaction obtains performed polymer；Dispersing agent is added in performed polymer, adds carbonyl iron dust dispersion liquid, obtains lotion；And the pH of lotion is adjusted, it is stirred to react, obtains carbonyl iron dust wave absorbing agent.
Description
Technical field
The present invention relates to absorbing materials, more particularly, to a kind of carbonyl iron dust wave absorbing agent and preparation method thereof.
Background technique
Carbonyl iron dust is a kind of common wave absorbing agent, its magnetic conductivity with higher, in the Microwave Frequency for being higher than superhigh frequency band
It is a kind of excellent electromagnetic wave absorption agent with interior use, but there are many disadvantages, examples for the absorbing material based on carbonyl iron dust preparation
Such as, it in order to reach higher absorption intensity, needs to fill a large amount of carbonyl iron dust in the material, carbonyl iron dust is caused to be difficult to disperse
Among matrix, the decline of absorbing property and the loss of matrix mechanical property are further caused.In addition, made of carbonyl iron dust
Absorbing material is placed in air for a long time, and surface can adsorb oxygen in air and water and aoxidize carbonyl iron dust slowly, surface oxidation
Generation Fe2O3Or Fe3O4.Oxidation can wear off wave absorbing agent effective component, in turn result in being greatly reduced for absorbing property.
Summary of the invention
In order to solve problem above, the present invention uses resin microcapsule modification technology, by the method for in-situ polymerization,
The certain thickness resin shell of carbonyl iron dust Surface Creation, improves the absorbing property of carbonyl iron dust, and improve carbonyl iron
The adhesion strength of powder and rubber matrix improves the compatibility of the two, while the carbonyl iron dust tool of heat cured resin package
There is preferable inoxidizability.
The present invention provides a kind of methods for preparing carbonyl iron dust wave absorbing agent, comprising the following steps:
Carbonyl iron dust is added in organic solvent, adds dispersion solvent, disperses, obtains carbonyl iron dust dispersion liquid；By first
Aldehyde and melamine mixing, obtain mixed liquor, adjust the pH of the mixed liquor, insulation reaction obtains performed polymer；In the pre-polymerization
Dispersing agent is added in body, adds the carbonyl iron dust dispersion liquid, obtains lotion；And the pH of the lotion is adjusted, stirring is anti-
It answers, obtains carbonyl iron dust wave absorbing agent.
In above method, the dispersion solvent includes dioctyl phthalate, dibutyl phthalate and adjacent benzene
One of dicarboxylate is a variety of.
In above method, the mass ratio of the carbonyl iron dust, the organic solvent and the dispersion solvent are as follows: 90-
110:5-12:50-80。
In above method, the mass ratio of the formaldehyde and the melamine are as follows: 1~1.5:2~3.
In above method, the pH of the mixed liquor is adjusted to 8-9.
In above method, the temperature of the insulation reaction is 40-60 DEG C, and the time of the insulation reaction is 1-2h.
In above method, the dispersing agent includes that Sodium Polyacrylate and polyethylene glycol 200 (have purchased from Dow Chemical
One or both of limit company).
In above method, the mass ratio of the performed polymer, the dispersing agent and the carbonyl iron dust dispersion liquid is 110-
130:1-5:140-170。
In above method, the pH of the lotion is adjusted to 8-9.
In above method, the temperature being stirred to react is 80-100 DEG C, and the time being stirred to react is 1-2h.
The present invention also provides a kind of carbonyl iron dust wave absorbing agents prepared according to the above method.
The beneficial effect of carbonyl iron dust wave absorbing agent prepared by the method for the present invention is:
One, by resin microcapsule modified carbonyl iron powder, it can effectively improve the absorption intensity of wave absorbing agent, simultaneously because
Absorption peak can be used for the absorbing material of high frequency to high frequency (being greater than 4GHz) offset；
Two, wave absorbing agent of the invention has preferable dispersibility, can be improved the intensity and toughness of the absorbing material of preparation；
Three, due to the package of resin layer, the inoxidizability of wave absorbing agent is improved.
Specific embodiment
The following examples can make those skilled in the art that the present invention be more fully understood, but not limit in any way
The present invention.
Following number is mass parts.
The present invention use emulsion polymerization method, be utilized respectively carbonyl iron dust oiliness and resin it is aqueous, pass through control
Resin layer, is wrapped in the surface of carbonyl iron dust by suitable chemical reaction condition (that is, control reaction temperature and reaction time)；And
And the mass ratio by controlling reactant wraps up quality and Jacket thickness to control.
In the present invention, stably dispersing is improved as water-soluble organic solvent using isopropanol, ethyl alcohol and/acetone
Property, so that carbonyl iron dust preferably disperses；
Carbonyl iron dust is coated using thermosetting resin (performed polymer that formaldehyde and melamine are formed), improves carbonyl
While iron powder dispersibility, the inoxidizability of carbonyl iron dust is improved；
Using formaldehyde and melamine as capsule material, the insulation reaction 1- at a temperature of pH is adjusted to 8-9 and 40-60 DEG C
2h, obtained the performed polymer (that is, thermosetting resin) of microcapsules, lower pH (pH < 8) or temperature (40 DEG C of temperature <) and
Higher pH (pH > 9) or temperature (60 DEG C of temperature >) all cannot be such that formaldehyde and melamine preferably polymerize, and then cannot obtain
To the performed polymer of microcapsules；
Meanwhile performed polymer, dispersing agent and carbonyl iron that the present invention is 110-130:1-5:140-170 by using mass ratio
Powder dispersion liquid wraps up quality and Jacket thickness to control；Wherein, when the dosage of performed polymer is excessive, Jacket thickness can be made too thick
And the absorbing property of carbonyl iron dust wave absorbing agent is influenced, when the dosage of performed polymer is too small, then it cannot be completely coated with carbonyl iron dust；
And dispersing agent can be such that performed polymer and carbonyl iron dust dispersion liquid preferably disperses, conducive to the progress of reaction, when the use of dispersing agent
When measuring too small, dispersion effect is unobvious, when dispersant dosage is excessive, can hinder the progress of reaction；
In addition, being stirred to react 1-2h at a temperature of pH is adjusted to 8-9 and 80-100 DEG C, this is stirred to react the control of condition
Resin layer further such that is wrapped in the surface of carbonyl iron dust by the method for in-situ polymerization by system.
The present invention provides a kind of carbonyl iron dust wave absorbing agents and preparation method thereof, method includes the following steps:
90-110 parts of carbonyl irons are added in 5-12 parts of organic solvents (including but not limited to isopropanol, ethyl alcohol and acetone)
Powder adds 50-80 parts of dispersion solvents, and the ultrasonic disperse 1-3h under the power of 600-900W obtains carbonyl iron dust dispersion liquid；Its
In, dispersion solvent include one of dioctyl phthalate, dibutyl phthalate and diethyl phthalate or
It is a variety of.
By 40-60 parts of formaldehyde and 80-120 parts of melamines, the mixing in reaction vessel (such as beaker), obtains mixed liquor, uses
It is 8-9 that ammonium hydroxide, which adjusts pH of mixed, and 40-60 DEG C of insulation reaction 1-2h obtains performed polymer；
1-5 parts of dispersing agents (including but not limited to Sodium Polyacrylates and polyethylene glycol are added in 110-130 parts of performed polymers
200) it, stirs evenly, adds 140-170 parts of carbonyl iron dust dispersion liquids, stir and formed in the case where revolving speed is 1000-1400r/min
Stable lotion；And with the pH that ammonium hydroxide adjusts the lotion be 8-9,80-100 DEG C is stirred to react 1-2h, washing 3-5 times, with following
Ring ability of swimming multiplex vavuum pump filters, obtains the carbonyl iron dust wave absorbing agent of microencapsulation after 80-100 DEG C of dry 10-12h.
Embodiment 1
100 parts of carbonyl iron dusts are added in 10 parts of isopropanols, add 50 parts of dioctyl phthalates, ultrasonic disperse
2h obtains carbonyl iron dust dispersion liquid；
50 parts of formaldehyde and 100 parts of melamines are mixed, mixed liquor is obtained, adjusting pH of mixed with ammonium hydroxide is 8,45 DEG C of guarantors
Temperature reaction 1.5h, obtains performed polymer；
120 parts of performed polymers are weighed from the above performed polymer, and 2 parts of Sodium Polyacrylates are added in the performed polymer, stir evenly,
160 parts of carbonyl iron dust dispersion liquids are added, stirring forms stable lotion；And adjusting the pH of the lotion with ammonium hydroxide is 8,80 DEG C
It is stirred to react 1h, washing filters, obtains the carbonyl iron dust wave absorbing agent of microencapsulation after drying.
Embodiment 2
100 parts of carbonyl iron dusts are added in 9 parts of ethyl alcohol, add 70 parts of dioctyl phthalates, ultrasonic disperse 1.5h,
Obtain carbonyl iron dust dispersion liquid；
55 parts of formaldehyde and 110 parts of melamines are mixed, mixed liquor is obtained, adjusting pH of mixed with ammonium hydroxide is 9,50 DEG C of guarantors
Temperature reaction 1.5h, obtains performed polymer；
125 parts of performed polymers are weighed from the above performed polymer, and 3 parts of Sodium Polyacrylates are added in the performed polymer, stir evenly,
150 parts of carbonyl iron dust dispersion liquids are added, stirring forms stable lotion；And adjusting the pH of the lotion with ammonium hydroxide is 9,95 DEG C
It is stirred to react 1.5h, washing filters, obtains the carbonyl iron dust wave absorbing agent of microencapsulation after drying.
Embodiment 3
100 parts of carbonyl iron dusts are added in 5 parts of isopropanols, add 75 parts of dioctyl phthalates, ultrasonic disperse 2h,
Obtain carbonyl iron dust dispersion liquid；
45 parts of formaldehyde and 85 parts of melamines are mixed, mixed liquor is obtained, adjusting pH of mixed with ammonium hydroxide is 8.5,55 DEG C
Insulation reaction 1.5h, obtains performed polymer；
120 parts of performed polymers are weighed from the above performed polymer, and 4 parts of Sodium Polyacrylates are added in the performed polymer, stir evenly,
160 parts of carbonyl iron dust dispersion liquids are added, stirring forms stable lotion；And adjusting the pH of the lotion with ammonium hydroxide is 9,90 DEG C
It is stirred to react 1h, washing filters, obtains the carbonyl iron dust wave absorbing agent of microencapsulation after drying.
Embodiment 4
90 parts of carbonyl iron dusts are added in 5 parts of isopropanols, add 50 parts of dibutyl phthalates, ultrasonic disperse 1h,
Obtain carbonyl iron dust dispersion liquid；
40 parts of formaldehyde and 80 parts of melamines are mixed, mixed liquor is obtained, adjusting pH of mixed with ammonium hydroxide is 8,40 DEG C of guarantors
Temperature reaction 2h, obtains performed polymer；
110 parts of performed polymers are weighed from the above performed polymer, 1 part of polyethylene glycol 200 is added in the performed polymer, and stirring is equal
It is even, 140 parts of carbonyl iron dust dispersion liquids are added, stirring forms stable lotion；And adjusting the pH of the lotion with ammonium hydroxide is 8,
80 DEG C are stirred to react 2h, and washing filters, obtains the carbonyl iron dust wave absorbing agent of microencapsulation after drying.
Embodiment 5
110 parts of carbonyl iron dusts are added in 12 parts of isopropanols, add 80 parts of dibutyl phthalates and O-phthalic
Diethyl phthalate (mass ratio 1:1), ultrasonic disperse 3h obtain carbonyl iron dust dispersion liquid；
60 parts of formaldehyde and 120 parts of melamines are mixed, mixed liquor is obtained, adjusting pH of mixed with ammonium hydroxide is 9,60 DEG C of guarantors
Temperature reaction 1h, obtains performed polymer；
130 parts of performed polymers are weighed from the above performed polymer, and 5 parts of Sodium Polyacrylates are added in the performed polymer, stir evenly,
170 parts of carbonyl iron dust dispersion liquids are added, stirring forms stable lotion；And adjusting the pH of the lotion with ammonium hydroxide is 9,100
DEG C be stirred to react 1h, washing, filter, it is dry after obtain the carbonyl iron dust wave absorbing agent of microencapsulation.
Embodiment 6
105 parts of carbonyl iron dusts are added in 7 parts of acetone, add 75 parts of dioctyl phthalates, ultrasonic disperse 2h is obtained
To carbonyl iron dust dispersion liquid；
40 parts of formaldehyde and 120 parts of melamines are mixed, mixed liquor is obtained, adjusting pH of mixed with ammonium hydroxide is 8.5,60 DEG C
Insulation reaction 1h, obtains performed polymer；
130 parts of performed polymers are weighed from the above performed polymer, and 2 parts of Sodium Polyacrylates and polyethylene glycol are added in the performed polymer
200 (mass ratio 1:1), stir evenly, and add 150 parts of carbonyl iron dust dispersion liquids, and stirring forms stable lotion；And it uses
The pH that ammonium hydroxide adjusts the lotion is 9,80 DEG C and is stirred to react 1.5h, and washing filters, obtains the carbonyl iron dust of microencapsulation after drying
Wave absorbing agent.
The carbonyl iron dust wave absorbing agent that 8 parts of carbonyl iron dusts and embodiment 1 are prepared into embodiment 6 respectively is (that is, micro- glue
The carbonyl iron dust wave absorbing agent of encapsulated) it is heated in 50-60 DEG C of baking oven with 2 parts of paraffin, it takes out rapidly be mixed evenly later,
Thick solid is made and is filled into coaxial toroidal mold (mold outer diameter 7mm, internal diameter 3.04mm), 1-2mm is prepared respectively
The coaxial annulus for the carbonyl iron dust wave absorbing agent that thick carbonyl iron dust and embodiment 1 is prepared into embodiment 6, then use network
Vector analysis instrument measures complex dielectric permittivity and complex permeability respectively, is then emulated according to electromagnetic field transmission line theory by matlab
Calculate carbonyl iron dust and reflection damage in thickness 2mm of carbonyl iron dust wave absorbing agent that embodiment 1 is prepared into embodiment 6
Consumption is with frequency variation curve；And it is prepared using Particle Size Analyzer test carbonyl iron dust and embodiment 1 into embodiment 6
The partial size of carbonyl iron dust wave absorbing agent, test result is as follows shown in table 1:
Table 1
| Average grain diameter (μm) | It absorbs peak position (GHz) | Absorption peak (dB) | |
| Embodiment 1 | 2.15 | 4.12 | -8.21 |
| Embodiment 2 | 2.53 | 4.03 | -8.9 |
| Embodiment 3 | 3.3 | 4.05 | -10.2 |
| Embodiment 4 | 2.17 | 4.51 | -11.7 |
| Embodiment 5 | 2.92 | 4.07 | -10.8 |
| Embodiment 6 | 2.86 | 4.25 | -9.6 |
| Carbonyl iron dust | 1.52 | 2.95 | -7.2 |
The carbonyl iron dust wave absorbing agent prepared by the method for the present invention it can be seen from upper table 1, partial size increase from 1.52 μm
To 2.15 μm or more, show that thermosetting resin (performed polymer that formaldehyde and melamine are formed) layer is successfully wrapped in carbonyl iron dust table
Face, and thickness is coated about between 0.6 μm -1.5 μm；This is because the present invention controls packet by controlling the dosage of reactant
Wrap up in quality and Jacket thickness, wherein performed polymer, dispersing agent and carbonyl iron dust dispersion liquid mass ratio are 110-130:1-5:140-
170, when the dosage of performed polymer is excessive, Jacket thickness can be made too thick and influence the absorbing property of carbonyl iron dust wave absorbing agent, when
When the dosage of performed polymer is too small, then carbonyl iron dust cannot be completely coated with.
In addition, the absorption peak position of carbonyl iron dust wave absorbing agent prepared by the method for the present invention is to high-frequency mobile, from
It is even higher that 2.95GHz is moved to 4.03GHz, and absorption peak can be reduced to -8.21 even lower from -7.2dB, effectively increase
The absorbing property of the wave absorbing agent；This is because the present invention uses resin microcapsule modification technology, pass through the side of in-situ polymerization
Method improves the absorbing property of carbonyl iron dust, and make absorption peak in the certain thickness resin shell of carbonyl iron dust Surface Creation
To high frequency (being greater than 4GHz) offset.
It is pressed using the carbonyl iron dust wave absorbing agent that carbonyl iron dust and embodiment 1 are prepared into embodiment 6 with nitrile matrix
Ratio mixing according to 80:20 is sulfided into corresponding wave absorbing patch, using method commonly used in the art to corresponding wave absorbing patch
Mechanics Performance Testing is carried out, test result see the table below 2:
Table 2
| Tensile strength | Elongation at break | |
| Embodiment 1 | 9.2MPa | 72% |
| Embodiment 2 | 9.5MPa | 65% |
| Embodiment 3 | 8.9MPa | 76% |
| Embodiment 4 | 9.1MPa | 75% |
| Embodiment 5 | 9.2MPa | 73% |
| Embodiment 6 | 9.5MPa | 68% |
| Carbonyl iron dust | 4.2MPa | 33% |
From table 2 it can be seen that stretching slightly to can achieve and not wrap up by the carbonyl iron dust wave absorbing agent that resin layer wraps up
2 times of carbonyl iron dust are improved from the 4.2MPa of carbonyl iron dust to 8.9MPa or more, and elongation at break is also improved from 33% to 65%
More than；This is because resin package after the certain thickness resin shell of carbonyl iron dust Surface Creation, improve carbonyl iron dust and
The adhesion strength of rubber matrix improves the compatibility of the two, so that the carbonyl iron dust that embodiment 1 is prepared into embodiment 6
Wave absorbing agent disperses intensity and toughness more uniform, and then that can be improved the absorbing material of preparation with rubber matrix.
To sum up, carbonyl iron dust absorbing material prepared by the method for the present invention can be applied to absorbing material field, example
Such as wave absorbing patch, antiradar coatings.
It will be understood by those skilled in the art that above embodiments are only exemplary embodiments, without departing substantially from spirit of the invention
In the case where range, a variety of variations can be carried out, replaced and changed.
Claims (10)
1. a kind of method for preparing carbonyl iron dust wave absorbing agent, which comprises the following steps:
Carbonyl iron dust is added in organic solvent, adds dispersion solvent, disperses, obtains carbonyl iron dust dispersion liquid；
Formaldehyde and melamine are mixed, mixed liquor is obtained, adjusts the pH of the mixed liquor, insulation reaction obtains performed polymer；
Dispersing agent is added in the performed polymer, adds the carbonyl iron dust dispersion liquid, obtains lotion；
The pH for adjusting the lotion, is stirred to react, and obtains carbonyl iron dust wave absorbing agent.
2. the method according to claim 1 for preparing carbonyl iron dust wave absorbing agent, which is characterized in that the dispersion solvent includes
One of dioctyl phthalate, dibutyl phthalate and diethyl phthalate are a variety of, the dispersing agent
Including one or both of Sodium Polyacrylate and polyethylene glycol 200.
3. the method according to claim 1 for preparing carbonyl iron dust wave absorbing agent, which is characterized in that the carbonyl iron dust, institute
State the mass ratio of organic solvent and the dispersion solvent are as follows: 90-110:5-12:50-80.
4. the method according to claim 1 for preparing carbonyl iron dust wave absorbing agent, which is characterized in that the formaldehyde and described three
The mass ratio of poly cyanamid are as follows: 1~1.5:2~3.
5. the method according to claim 1 for preparing carbonyl iron dust wave absorbing agent, which is characterized in that the pH tune of the mixed liquor
Section is 8-9.
6. the method according to claim 1 for preparing carbonyl iron dust wave absorbing agent, which is characterized in that the temperature of the insulation reaction
Degree is 40-60 DEG C, and the time of the insulation reaction is 1-2h.
7. the method according to claim 1 for preparing carbonyl iron dust wave absorbing agent, which is characterized in that the performed polymer, described
The mass ratio of dispersing agent and the carbonyl iron dust dispersion liquid is 110-130:1-5:140-170.
8. the method according to claim 1 for preparing carbonyl iron dust wave absorbing agent, which is characterized in that the pH of the lotion is adjusted
For 8-9.
9. the method according to claim 1 for preparing carbonyl iron dust wave absorbing agent, which is characterized in that the temperature being stirred to react
Degree is 80-100 DEG C, and the time being stirred to react is 1-2h.
10. a kind of carbonyl iron dust wave absorbing agent of method preparation according to claim 1 to 9.
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| CN116218249A (en) * | 2022-12-01 | 2023-06-06 | 南京信息工程大学 | Preparation method of thermoplastic elastomer-based flexible electromagnetic wave absorption film |
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Application publication date: 20190611 |