CN109575425A - Absorbing material and preparation method thereof - Google Patents
Absorbing material and preparation method thereof Download PDFInfo
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- CN109575425A CN109575425A CN201710896497.3A CN201710896497A CN109575425A CN 109575425 A CN109575425 A CN 109575425A CN 201710896497 A CN201710896497 A CN 201710896497A CN 109575425 A CN109575425 A CN 109575425A
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- carbonyl iron
- silane coupling
- carbon fiber
- modified
- coupling agent
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
- C08K7/06—Elements
Abstract
The present invention provides absorbing material and preparation method thereof, preparation method includes: that carbon fiber is placed in the first silane coupling agent to impregnate, and is stirred, dry, obtains modified carbon fiber；Carbonyl iron dust is mixed with the second silane coupling agent, is uniformly dispersed carbonyl iron dust, is reacted, filtering washs and dry, modified carbonyl iron powder is made；Polypropylene is warming up to the first temperature under stirring conditions, melts polypropylene, modified carbon fiber and modified carbonyl iron powder is added, is mixed evenly；It is hot-forming, obtain absorbing material.The present invention provides the absorbing materials with improved wave-absorbing effect and mechanical property.
Description
Technical field
The present invention relates to absorbing material, more particularly, to carbon fiber/carbonyl iron dust polypropylene electromagnetic-wave absorbent and its
Preparation method.
Background technique
Carbonyl iron dust is widely used in absorbing material field, is a kind of typical with relatively high complex permeability
Magnetic loss type absorbing material.The Composite of metal fine powder electromagnetic wave absorbing material is the direction of future development.However, iron powder is in resin
It is easy to reunite in mixing, dispersion is uneven.
Carbon fiber potting resin material can make composite material obtain good mechanical property and electric conductivity, still
Wave-absorbing effect is unobvious.In addition, carbon fiber surface is smooth, surface-active is low, with bad adhesion when resin-bonded, and then influence to inhale
The mechanical property of wave material.
Summary of the invention
The present invention provides a kind of carbon fiber/carbonyl iron dust polypropylene electromagnetic-wave absorbents, by the way that good absorption effect is added
Carbonyl iron dust filler, improve the shield effectiveness of absorbing material.In addition, being modified to carbonyl iron dust, to improve carbonyl iron
Dispersing uniformity of the powder in resin.In addition, handled using silane coupling agent carbon fiber surface, improve carbon fiber with
The caking property of resin.
The present invention provides a kind of methods for preparing absorbing material, comprising: carbon fiber is placed in the first silane coupling agent
Middle immersion is stirred, dry, obtains modified carbon fiber；Carbonyl iron dust is mixed with the second silane coupling agent, makes the carbonyl iron dust
It is uniformly dispersed, reacts, filtering washs and dry, modified carbonyl iron powder is made；Polypropylene is warming up under stirring conditions
First temperature, melts polypropylene, and the modified carbon fiber and the modified carbonyl iron powder is added, is mixed evenly；Hot pressing
Molding, obtains the absorbing material.
In the above-mentioned methods, wherein the weight of first silane coupling agent is the 0.5%- of the weight of the carbon fiber
2%.
In the above-mentioned methods, wherein the weight of second silane coupling agent is the 4%- of the weight of the carbonyl iron dust
6%.
In the above-mentioned methods, wherein first silane coupling agent and second silane coupling agent are identical or different.
In the above-mentioned methods, wherein the time that the carbonyl iron dust is reacted with second silane coupling agent is 40-
60min。
In the above-mentioned methods, wherein the weight ratio of the polypropylene, the modified carbon fiber and the modified carbonyl iron powder
For 6-8:1-2:1-3.
In the above-mentioned methods, wherein the hot-forming temperature is 180 DEG C -210 DEG C, pressure 12-15MPa.
In the above-mentioned methods, wherein further include being vented repeatedly during described hot-forming.
In the above-mentioned methods, wherein first temperature is 170 DEG C -190 DEG C.
In the above-mentioned methods, wherein first silane coupling agent and second silane coupling agent include A-1100,
A-187's and A-172 is one or more.
The present invention also provides the absorbing materials prepared by the above method.
The present invention by addition carbonyl iron dust and is modified carbonyl iron dust, improves carbonyl iron dust in resin material
In dispersion, improve the wave-absorbing effect of absorbing material.In addition, the present invention improves carbon fiber by being modified to carbon fiber
The adhesive property of dimension and resin material, to further improve the mechanical property of absorbing material.
Specific embodiment
Carbon fiber of the invention/carbonyl iron dust polypropylene electromagnetic-wave absorbent can be prepared by the following method: weigh silicon
Alkane coupling agent and carbon fiber, the weight of silane coupling agent are the 0.5%-2% of carbon fiber, and carbon fiber is placed in silane coupling agent
Middle immersion treatment stirs 2-4 hours to be modified to carbon fiber, is then placed into 60 DEG C of -80 DEG C of dryings in vacuum oven
6-8 hours spare.Carbonyl iron dust is mixed with silane coupler solution, the weight of silane coupling agent is the 4%- of carbonyl iron dust
6%, then (for example, ultrasonic disperse) will be dispersed at mixed solution in a water bath 40 DEG C -60 DEG C, it is evenly dispersed in iron powder
In solution, reaction 40-60min or so repeatedly washs by reactant filtering, with deionized water, is dry, being made organosilane-modified
Surface amination carbonyl iron dust；
It takes the pp material of 60-80 parts by weight to be placed in blender and is warming up to 170 DEG C -190 DEG C, it is completely molten to polypropylene
After changing uniformly, the modified carbon fiber of 10-20 parts by weight is taken to be placed in blender, 20-40min is mixed, after mixing
It takes the modified carbonyl iron dust of 10-30 parts by weight to be placed in blender, is mixed 1-2 hours, keeps filler abundant with resin
It is mixed evenly, mixing is divided into frustillatum, cooling under room temperature after mixing；
It is hot-forming with a thickness of 3mm, size under 180 DEG C -200 DEG C of temperature, the pressure of 12MPa-15MPa on press
For the plate of 300*300mm, it is vented repeatedly in hot pressing, it is ensured that in plate the defects of bubble-free.
In the present invention, silane coupling agent includes A-1100 (gamma-aminopropyl-triethoxy-silane), A-187 (γ-shrink
Glycerol ether oxygen propyl trimethoxy silicane) and A-172's (vinyl-three (2- methoxy ethoxy) silane) is one or more.
It is illustrated below with reference to specific embodiment, to better understand the invention.
Embodiment 1
Silane coupling A -1100 and carbon fiber are weighed, the dosage of silane coupling A -1100 is the 2% of carbon fiber, by carbon
Fiber is placed in immersion treatment in silane coupling A -1100, is handled 3 hours with mixing plant, is then placed into vacuum oven
In 60 DEG C drying 8 hours it is spare；Carbonyl iron dust is modified with wet process, by the solution of carbonyl iron dust and silane coupling A -1100
Mixing, the dosage of silane coupling A -1100 is the 6% of carbonyl iron dust quality, then will be carried out at mixed solution in a water bath 40 DEG C
Ultrasonic disperse is evenly dispersed in iron powder in solution, and reaction 40min or so is repeatedly washed by reactant filtering, with deionized water
It washs, dry, the carbonyl iron dust of organosilane-modified surface amination is made.
It takes the pp material of 80 parts by weight to be placed in blender and is warming up to 180 DEG C, after polypropylene is completely melt uniformly,
Take 10 it is part by weight modified after carbon fiber be placed in blender, be mixed 30min, the modified of 10 parts by weight is taken after mixing
Carbonyl iron dust be placed in blender, be mixed 1 hour, make filler (modified carbon fiber and modified carbonyl iron dust)
It is sufficiently mixed and stirs evenly with resin, mixing is divided into frustillatum, cooling under room temperature after mixing.
With 190 DEG C on press, pressure 12MPa is hot-forming with a thickness of 3mm, the plate having a size of 300*300mm, hot pressing
It is vented repeatedly in the process, it is ensured that in plate the defects of bubble-free.
Embodiment 2
Silane coupling A -187 and carbon fiber are weighed, the dosage of silane coupling A -187 is the 1% of carbon fiber, by carbon fiber
Dimension is placed in immersion treatment in silane coupling A -187, is handled 3 hours with mixing plant, is then placed into vacuum oven
70 DEG C drying 6 hours it is spare.Carbonyl iron dust is modified with wet process, and carbonyl iron dust and the solution of silane coupling A -1100 are mixed
It closes, the dosage of silane coupling A -1100 is the 5% of carbonyl iron dust quality, then will be surpassed at mixed solution in a water bath 50 DEG C
Sound dispersion, is evenly dispersed in iron powder in solution, and reaction 50min or so is repeatedly washed by reactant filtering, with deionized water
It washs, dry, the carbonyl iron dust of organosilane-modified surface amination is made.
It takes 70 parts of pp material to be placed in blender and is warming up to 180 DEG C, after polypropylene is completely melt uniformly, take 15
The modified carbon fiber of part is placed in blender, and 25min is mixed, 15 parts of modified carbonyl iron dusts is taken to be placed in after mixing
In blender, it is mixed 1 hour, is sufficiently mixed filler with resin and stirs evenly, be after mixing divided into mixing small
Bulk, it is cooling under room temperature.
With 180 DEG C on press, pressure 15MPa is hot-forming with a thickness of 3mm, the plate having a size of 300*300mm, hot pressing
It is vented repeatedly in the process, it is ensured that in plate the defects of bubble-free.
Embodiment 3
Silane coupling A -172 and carbon fiber are weighed, the dosage of silane coupling A -172 is the 0.5% of carbon fiber, by carbon
Fiber is placed in immersion treatment in silane coupling A -172, is handled 2.5 hours with mixing plant, is then placed into vacuum drying
In case 80 DEG C drying 6 hours it is spare.Carbonyl iron dust is modified with wet process, by the molten of carbonyl iron dust and silane coupling A -172
Liquid mixing, the dosage of silane coupling A -172 are the 5% of carbonyl iron dust quality, then by mixed solution in a water bath 60 DEG C into
Row ultrasonic disperse, is evenly dispersed in iron powder in solution, and reactant is filtered, is multiple with deionized water by reaction 60min or so
Washing, drying, are made the carbonyl iron dust of organosilane-modified surface amination.
It takes 70 parts of pp material to be placed in blender and is warming up to 170 DEG C, after polypropylene is completely melt uniformly, take 20
The modified carbon fiber of part is placed in blender, and 30min is mixed, 10 parts of modified carbonyl iron dusts is taken to be placed in after mixing
In blender, it is mixed 1 hour, is sufficiently mixed filler with resin and stirs evenly, be after mixing divided into mixing small
Bulk, it is cooling under room temperature.
With 200 DEG C on press, pressure 15MPa is hot-forming with a thickness of 3mm, the plate having a size of 300*300mm, hot pressing
It is vented repeatedly in the process, it is ensured that in plate the defects of bubble-free.
Embodiment 4
Silane coupling A -1100 and carbon fiber are weighed, the dosage of silane coupling A -1100 is the 1% of carbon fiber, by carbon
Fiber is placed in immersion treatment in silane coupling A -1100, is handled 2 hours with mixing plant, is then placed into vacuum oven
In 70 DEG C drying 6 hours it is spare.Carbonyl iron dust is modified with wet process, by the solution of carbonyl iron dust and silane coupling A -172
Mixing, the dosage of silane coupling A -172 is the 5% of carbonyl iron dust quality, then will be carried out at mixed solution in a water bath 60 DEG C
Ultrasonic disperse is evenly dispersed in iron powder in solution, and reaction 50min or so is repeatedly washed by reactant filtering, with deionized water
It washs, dry, the carbonyl iron dust of organosilane-modified surface amination is made.
It takes 70 parts of pp material to be placed in blender and is warming up to 190 DEG C, after polypropylene is completely melt uniformly, take 10
The modified carbon fiber of part is placed in blender, and 20min is mixed, 20 parts of modified carbonyl iron dusts is taken to be placed in after mixing
In blender, it is mixed 1 hour, is sufficiently mixed filler with resin and stirs evenly, be after mixing divided into mixing small
Bulk, it is cooling under room temperature.
With 210 DEG C on press, pressure 13MPa is hot-forming with a thickness of 3mm, the plate having a size of 300*300mm, hot pressing
It is vented repeatedly in the process, it is ensured that in plate the defects of bubble-free.
Embodiment 5
Silane coupling A -172 and carbon fiber are weighed, the dosage of silane coupling A -172 is the 1% of carbon fiber, by carbon fiber
Dimension is placed in immersion treatment in silane coupling A -172, is handled 3 hours with mixing plant, is then placed into vacuum oven
70 DEG C drying 6 hours it is spare.Carbonyl iron dust is modified with wet process, and carbonyl iron dust and the solution of silane coupling A -172 are mixed
It closes, the dosage of silane coupling A -172 is the 4% of carbonyl iron dust quality, then will be surpassed at mixed solution in a water bath 60 DEG C
Sound dispersion, is evenly dispersed in iron powder in solution, and reaction 60min or so is repeatedly washed by reactant filtering, with deionized water
It washs, dry, the carbonyl iron dust of organosilane-modified surface amination is made.
It takes 60 parts of pp material to be placed in blender and is warming up to 185 DEG C, after polypropylene is completely melt uniformly, take 20
The modified carbon fiber of part is placed in blender, and 40min is mixed, 20 parts of modified carbonyl iron dusts is taken to be placed in after mixing
In blender, it is mixed 1.5 hours, is sufficiently mixed filler with resin and stirs evenly, be after mixing divided into mixing
Small bulk, it is cooling under room temperature.
With 190 DEG C on press, pressure 14MPa is hot-forming with a thickness of 3mm, the plate having a size of 300*300mm, hot pressing
It is vented repeatedly in the process, it is ensured that in plate the defects of bubble-free.
Embodiment 6
Silane coupling A -1100 and carbon fiber are weighed, the dosage of silane coupling A -1100 is the 1% of carbon fiber, by carbon
Fiber is placed in immersion treatment in silane coupling A -1100, is handled 4 hours with mixing plant, is then placed into vacuum oven
In 70 DEG C drying 6 hours it is spare.Carbonyl iron dust is modified with wet process, by the solution of carbonyl iron dust and silane coupling A -1100
Mixing, the dosage of silane coupling A -1100 is the 6% of carbonyl iron dust quality, then will be carried out at mixed solution in a water bath 60 DEG C
Ultrasonic disperse is evenly dispersed in iron powder in solution, and reaction 60min or so is repeatedly washed by reactant filtering, with deionized water
It washs, dry, organosilane-modified surface amination carbonyl iron dust is made.
It takes 60 parts of pp material to be placed in blender and is warming up to 180 DEG C, after polypropylene is completely melt uniformly, take 10
The modified carbon fiber of part is placed in blender, and 30min is mixed, 30 parts of modified carbonyl iron dusts is taken to be placed in after mixing
In blender, it is mixed 2 hours, is sufficiently mixed filler with resin and stirs evenly, be after mixing divided into mixing small
Bulk, it is cooling under room temperature.
With 190 DEG C on press, pressure 15MPa is hot-forming with a thickness of 3mm, the plate having a size of 300*300mm, hot pressing
It is vented repeatedly in the process, it is ensured that in plate the defects of bubble-free.
The reflection loss and mechanical property of the absorbing material of above-described embodiment are measured using method commonly used in the art, instead
It penetrates rate to measure using SFL-I Albedometer, the mechanical property of sample test material is cut according to GB/T1040.2-2006 standard
Can, testing equipment: universal material stretching-machine.1~18GHz of carbon fiber obtained/carbonyl iron dust polypropylene electromagnetic-wave absorbent
Under reflection loss maximum value, the measurement result of tensile strength and elongation at break it is as shown in table 1 below.
Table 1
As shown in Table 1, the present invention by addition carbonyl iron dust and is modified carbonyl iron dust, improves carbonyl iron dust
Dispersion in resin material improves the wave-absorbing effect of absorbing material, the maximum reflection damage in 1~18GHz frequency range
Consumption value is less than or equal to -15dB, hence it is evident that better than-the 10dB of conventional absorbing material.In addition, the present invention is by changing carbon fiber
Property, the adhesive property of carbon fiber and resin material is improved, to further improve the mechanical property of absorbing material, is stretched strong
For degree in 36MPa or more, elongation at break is significantly better than that conventional absorbing material is less than the tensile strength of 30MPa 55% or more
With the elongation at break less than 50%.
The present invention, which has been made, meets thin, light, wide, strong demand absorbing material, and the decaying improved to electromagnetic wave is inhaled
It receives, can be applied to the numerous areas such as aerospace, ship naval vessels, radar antenna and electronic shield.
Claims (11)
1. a kind of method for preparing absorbing material characterized by comprising
Carbon fiber is placed in the first silane coupling agent and is impregnated, is stirred, it is dry, obtain modified carbon fiber；
Carbonyl iron dust is mixed with the second silane coupling agent, is uniformly dispersed the carbonyl iron dust, react, filtering, washing and
It is dry, modified carbonyl iron powder is made；
Polypropylene is warming up to the first temperature under stirring conditions, melts polypropylene, the modified carbon fiber and institute is added
Modified carbonyl iron powder is stated, is mixed evenly；
It is hot-forming, obtain the absorbing material.
2. the method according to claim 1, wherein the weight of first silane coupling agent is the carbon fiber
Weight 0.5%-2%.
3. the method according to claim 1, wherein the weight of second silane coupling agent is the carbonyl iron
The 4%-6% of the weight of powder.
4. the method according to claim 1, wherein first silane coupling agent and described second silane coupled
Agent is identical or different.
5. the method according to claim 1, wherein the carbonyl iron dust is reacted with second silane coupling agent
Time be 40-60min.
6. the method according to claim 1, wherein the polypropylene, the modified carbon fiber and the modification
The weight ratio of carbonyl iron dust is 6-8:1-2:1-3.
7. the method according to claim 1, wherein the hot-forming temperature be 180 DEG C -210 DEG C, pressure
For 12-15MPa.
8. the method according to claim 1, wherein further including being arranged repeatedly during described hot-forming
Gas.
9. the method according to claim 1, wherein first temperature is 170 DEG C -190 DEG C.
10. the method according to claim 1, wherein first silane coupling agent and second silane are even
Joining agent includes the one or more of A-1100, A-187 and A-172.
11. the absorbing material of method preparation according to claim 1 to 10.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710896497.3A CN109575425A (en) | 2017-09-28 | 2017-09-28 | Absorbing material and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710896497.3A CN109575425A (en) | 2017-09-28 | 2017-09-28 | Absorbing material and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111333961A (en) * | 2020-04-24 | 2020-06-26 | 苏州申赛新材料有限公司 | Wave-absorbing material and preparation method thereof |
| CN114250630A (en) * | 2020-09-23 | 2022-03-29 | 湖南博翔新材料有限公司 | Pyrolytic carbonyl iron coating carbon fiber and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101362390A (en) * | 2008-09-28 | 2009-02-11 | 北京理工大学 | Wide band electromagnetic wave-shielded polyethylene compound film containing carbonyl iron powder and preparation method thereof |
| CN101735501A (en) * | 2008-11-20 | 2010-06-16 | 宁波山泉建材有限公司 | Composite material with radar absorbing function and preparation method |
| 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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2017
- 2017-09-28 CN CN201710896497.3A patent/CN109575425A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101362390A (en) * | 2008-09-28 | 2009-02-11 | 北京理工大学 | Wide band electromagnetic wave-shielded polyethylene compound film containing carbonyl iron powder and preparation method thereof |
| CN101735501A (en) * | 2008-11-20 | 2010-06-16 | 宁波山泉建材有限公司 | Composite material with radar absorbing function and preparation method |
| 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 |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111333961A (en) * | 2020-04-24 | 2020-06-26 | 苏州申赛新材料有限公司 | Wave-absorbing material and preparation method thereof |
| CN114250630A (en) * | 2020-09-23 | 2022-03-29 | 湖南博翔新材料有限公司 | Pyrolytic carbonyl iron coating carbon fiber and preparation method thereof |
| CN114250630B (en) * | 2020-09-23 | 2023-08-01 | 湖南博翔新材料有限公司 | Pyrolytic carbonyl iron coating carbon fiber and preparation method thereof |
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