CN107857852A - Polyurethane wave-absorbing material and preparation method thereof - Google Patents
Polyurethane wave-absorbing material and preparation method thereof Download PDFInfo
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- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
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- C08J2201/00—Foams characterised by the foaming process
- C08J2201/04—Foams characterised by the foaming process characterised by the elimination of a liquid or solid component, e.g. precipitation, leaching out, evaporation
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Abstract
The invention provides a kind of polyurethane wave-absorbing material, wherein, it is obtained by the aggregated reaction of component of following mass parts：100 parts of PPG, 20~70 parts of toluene di-isocyanate(TDI), 0.01~0.5 part of nano carbon sol, 10~20 parts of deionized water, 5~30 parts of methyl-phosphoric acid dimethyl ester, 2~10 parts of carboxyl multi-walled carbon nanotube, 10~40 parts of ferroso-ferric oxide, 1~10 part of Firebrake ZB, 0.02~0.4 part of stannous octoate, 0.03~0.6 part of triethylene diamine, 0.2~3 part of organic silicon surfactant, 1~10 part of sodium acid carbonate.Above-mentioned polyurethane wave-absorbing material provided by the invention has the characteristics that low cigarette, low toxicity, absorption frequency distribution that is fire retardant, absorbing ripple are wide.The present invention also provides a kind of preparation method of above-mentioned polyurethane wave-absorbing material.
Description
Technical field
The invention belongs to technical field of function materials, and in particular to a kind of polyurethane wave-absorbing material and preparation method thereof.
Background technology
Absorbing material, it is to refer to be projected onto the electromagnetic wave on its surface largely to absorb and change into the energy of other forms
Amount and almost unreflected material.With the development of modern science and technology, influence of the electromagenetic wave radiation to environment increasingly increases.
Airport, airplane flight are overdue because Electromagnetic Interference can not take off；In hospital, mobile phone can often disturb various electronic instrument for diagnosing and curing diseases
The normal work of device.Other electromagnetic radiation causes wound directly or indirectly by fuel factor, non-thermal effect, cumulative effect to human body
Evil.Therefore, electromagnetic pollution is administered, finds a kind of material that can be kept out and weaken electromagenetic wave radiation --- absorbing material, it has also become
One big problem of material science.
Polyurethane foam has that porous, relative density is small, and heatproof, ageing-resistant, anti-organic solvent corrode, easily shaping
The features such as processing, it is widely used in absorbing material.At present mainly by the way that wave absorbing agent is added into hard polyurethane foam system,
It is re-introduced into mould and reacts foaming, or flexible polyurethane foams are cut into predetermined shape, impregnates wave absorbing agent solution to make
Standby polyurethane foam composite wave-suction material, these materials have that complex manufacturing technology, function are single, inhale ripple auxiliary agent and be easy to come off,
The defects of inflammable.
Chinese patent CN200910029840.X " foamed high resilience polyurethane wave-absorbing material and preparation method thereof " is open
A kind of polyurethane wave-absorbing material prepared using the raw materials such as auxiliary agent, fire retardant are absorbed.But the material has that size is big, makes work
The defects of skill complexity.It is to inhale ripple material that raising fire resistance, manufacture craft are simple while how improving absorbing property, reduce pollution
Expect the key issue of development.
The content of the invention
In view of this, the present invention is above-mentioned to solve it is necessory to provide a kind of polyurethane wave-absorbing material and preparation method thereof
Problem.
The present invention provides a kind of polyurethane wave-absorbing material, and it is obtained by the aggregated reaction of component of following mass parts：Polyethers
100 parts of polyalcohol, 20~70 parts of toluene di-isocyanate(TDI), 0.01~0.5 part of nano carbon sol, 10~20 parts of deionized water, first
5~30 parts of base dimethyl phosphate, 2~10 parts of carboxyl multi-walled carbon nanotube, 10~40 parts of ferroso-ferric oxide, 1~10 part of Firebrake ZB,
0.02~0.4 part of stannous octoate, 0.03~0.6 part of triethylene diamine, 0.2~3 part of organic silicon surfactant, sodium acid carbonate 1
~10 parts.
Wherein, the polyether polyol hydroxyl value is 30~60mgKOH/g.The isocyanates of the toluene di-isocyanate(TDI)
Index is 0.60~1.15.
Based on above-mentioned, the polyurethane wave-absorbing material is obtained by the aggregated reaction of component of following mass parts：Polyether polyols
100 parts of alcohol, 40~50 parts of toluene di-isocyanate(TDI), 0.1~0.3 part of nano carbon sol, 13~17 parts of deionized water, methyl acid phosphate
12~23 parts of dimethyl ester, 4~8 parts of carboxyl multi-walled carbon nanotube, 20~30 parts of ferroso-ferric oxide, 5~6 parts of Firebrake ZB, octanoic acid are sub-
0.08~0.3 part of tin, 0.12~0.45 part of triethylene diamine, 1~2 part of organic silicon surfactant, 5~7 parts of sodium acid carbonate.
The present invention also provides a kind of preparation method of above-mentioned polyurethane wave-absorbing material, and it comprises the following steps：
Raw material mixes：PPG, methyl-phosphoric acid dimethyl ester, nano carbon sol, ferroso-ferric oxide, Firebrake ZB, octanoic acid is sub-
Tin, triethylene diamine, deionized water, organic silicon surfactant are stirred at room temperature uniformly, then handled through ultrasonic disperse
To first mixture；
Reaction foaming：First toluene di-isocyanate(TDI) is added into the first mixture and be stirred by ultrasonic 5~10 minutes, add
Carboxyl CNT and sodium acid carbonate, mould is then poured into rapidly and carries out room temperature foaming 30~90 minutes, absorbing material is obtained and coagulates
Glue；
Freeze-drying：The absorbing material gel be freeze-dried and produces the polyurethane wave-absorbing material.
Included based on the step of above-mentioned, the reaction is foamed：In the presence of ultrasonic agitation, first by toluene di-isocyanate(TDI)
5~10 minutes in the first mixture is added under conditions of heating while stirring, carboxyl CNT and carbon are added
Sour hydrogen sodium；Then mould is poured into rapidly and carries out room temperature foaming 30~90 minutes, obtains the absorbing material gel.
Based on above-mentioned, in the step of raw material mixes, the ultrasonic disperse processing is carried out in a water bath.
Include based on above-mentioned, the step of the freeze-drying：First the absorbing material gel is freezed 10~70 hours, it is cold
It is 5~50 DEG C below mixed solution freezing point temperature to freeze temperature；Then by the mixed solution after freezing further in -10~-100
DEG C low-temp low-pressure is dried 24~96 hours, and pressure is 0.1~1kPa；Finally by the dried mixed solution of low-temp low-pressure in 60~
100 DEG C solidify 4~12 hours.
Compared with prior art, polyurethane wave-absorbing material provided by the invention uses methyl-phosphoric acid dimethyl ester and Firebrake ZB phase
With reference to being allowed to play fire-retardant synergy so that the polyurethane wave-absorbing material has the characteristics that low cigarette, low toxicity, fire retardant, and
The fire resistance of the material reaches HF-1 levels；Sodium acid carbonate produces bubble with the reaction of carboxyl CNT, while coordinates freezing dry
Dry technology removes the deionized water in the absorbing material gel so that and the polyurethane wave-absorbing material of preparation has loose structure,
Larger specific surface area, in addition, nano carbon sol and multi-walled carbon nanotube have larger an adsorptivity and electric conductivity, then with four oxygen
Change three-iron to coordinate so that the polyurethane wave-absorbing material has higher wave absorbing efficiency, and absorption frequency distribution is wide, suitable for inhaling ripple
Stealthy field.Further, since nano carbon sol and multi-walled carbon nanotube have preferable electric conductivity, and it is evenly dispersed in poly-
In urethane matrix and good conductive network is formed, the electric property for preparing gained compound polyurethane material is improved and stably, exceeded
It is low to ooze value.The present invention is combined using chemical foaming technology and orientation Freeze Drying Technique inhales ripple material to prepare the polyurethane
Material, preparation technology is simple, small investment, and production efficiency is high, environment-friendly.
Embodiment
Below by embodiment, technical scheme is described in further detail.
Embodiment 1
The embodiment of the present invention provides a kind of polyurethane wave-absorbing material, and it is obtained by the aggregated reaction of component of following mass parts：It is poly-
100 parts of ethoxylated polyhydric alcohol, 20 parts of toluene di-isocyanate(TDI), 0.01 part of nano carbon sol, 10 parts of deionized water, methyl-phosphoric acid dimethyl ester
5 parts, 2 parts of carboxyl multi-walled carbon nanotube, 10 parts of ferroso-ferric oxide, 1 part of Firebrake ZB, 0.02 part of stannous octoate, triethylene diamine
0.03 part, 0.2 part of organic silicon surfactant, 1 part of sodium acid carbonate.
The embodiment of the present invention also provides a kind of preparation method of above-mentioned polyurethane wave-absorbing material, and it comprises the following steps：
Raw material mixes：Above-mentioned mass parts, by PPG, methyl-phosphoric acid dimethyl ester, nano carbon sol, ferroso-ferric oxide, boron
Sour zinc, stannous octoate, triethylene diamine, deionized water, organic silicon surfactant are stirred at room temperature uniformly, then through ultrasound
Decentralized processing obtains first mixture；
Reaction foaming：In the presence of ultrasonic agitation, first toluene di-isocyanate(TDI) is added under conditions of heating while stirring
Into the first mixture 5~10 minutes, carboxyl CNT and sodium acid carbonate are added；Then mould progress is poured into rapidly
Room temperature foams 30 minutes, obtains absorbing material gel；
Freeze-drying：First the absorbing material gel is freezed 10 hours, cryogenic temperature is 5 below mixed solution freezing point temperature
℃；Then the mixed solution after freezing is further dried 24 hours in -10 DEG C of low-temp low-pressures, pressure is 0.1 kPa；Finally will
The dried mixed solution of low-temp low-pressure solidifies 12 hours in 60 DEG C, obtains above-mentioned polyurethane wave-absorbing material.
Performance test
Absorbing property detection method：It is 3cm × 3cm that above-mentioned polyurethane wave-absorbing material is cut into area, and thickness is 4 mm square
Shape sheet sample, and the very smooth aluminium foil of layer of surface is sticked on a side surface, using digital vector Network Analyzer
The microwave reflection rate curve of (8722ET types) test above-mentioned sample in 4~20 ghz bands.It will detect, absorbing property is in 4GHz
It is less than -30 db in~20GHz frequency ranges.
Fire resistance detection method：According to GB/T 8332-2008 foamed plastics combustibility test method horizontal firing methods
Detected to above-mentioned.After testing, the fire resistance of above-mentioned polyurethane wave-absorbing material reaches HF-1 levels.
Embodiment 2
The embodiment of the present invention provides a kind of polyurethane wave-absorbing material and obtained by the aggregated reaction of component of following mass parts：Polyethers is more
First 100 parts of alcohol, 30 parts of toluene di-isocyanate(TDI), 0.1 part of nano carbon sol, 13 parts of deionized water, 12 parts of methyl-phosphoric acid dimethyl ester,
4 parts of carboxyl multi-walled carbon nanotube, 20 parts of ferroso-ferric oxide, 5 parts of Firebrake ZB, 0.08 part of stannous octoate, 0.12 part of triethylene diamine,
1 part of organic silicon surfactant, 5 parts of sodium acid carbonate.
The embodiment of the present invention also provides a kind of preparation method of above-mentioned polyurethane wave-absorbing material, the preparation method and embodiment
1 preparation method provided is essentially identical, and difference is：
Reaction foaming：Room temperature foamed time in the step is 60 minutes；
Freeze-drying：The step includes first freezing the absorbing material gel 30 hours, and cryogenic temperature solidifies for mixed solution
15 DEG C below point temperature；Then the mixed solution after freezing is further dried 48 hours in -30 DEG C of low-temp low-pressures, pressure is
0.3 kPa；Finally the dried mixed solution of low-temp low-pressure is solidified 10 hours in 70 DEG C, above-mentioned polyurethane is obtained and inhales ripple material
Material.
Performance test
Using the identical method with being provided in embodiment 1, the absorption ripple of the polyurethane wave-absorbing material provided above-described embodiment
Performance and fire resistance are detected, and testing result is：Absorbing property is less than -37 db in 4GHz~20GHz frequency ranges,
The fire resistance of above-mentioned polyurethane wave-absorbing material reaches HF-1 levels.
Embodiment 3
The embodiment of the present invention provides a kind of polyurethane wave-absorbing material, and it is obtained by the aggregated reaction of component of following mass parts：It is poly-
100 parts of ethoxylated polyhydric alcohol, 40 parts of toluene di-isocyanate(TDI), 0.2 part of nano carbon sol, 15 parts of deionized water, methyl-phosphoric acid dimethyl ester
18 parts, 6 parts of carboxyl multi-walled carbon nanotube, 25 parts of ferroso-ferric oxide, 6 parts of Firebrake ZB, 0.2 part of stannous octoate, triethylene diamine 0.3
Part, 1.6 parts of organic silicon surfactant, 6 parts of sodium acid carbonate.
The embodiment of the present invention also provides a kind of preparation method of above-mentioned polyurethane wave-absorbing material, the preparation method and embodiment
1 preparation method provided is essentially identical, and difference is：
Reaction foaming：Room temperature foamed time in the step is 60 minutes；
Freeze-drying：The step includes first freezing the absorbing material gel 40 hours, and cryogenic temperature solidifies for mixed solution
30 DEG C below point temperature；Then the mixed solution after freezing is further dried 60 hours in -50 DEG C of low-temp low-pressures, pressure is
0.6 kPa；Finally the dried mixed solution of low-temp low-pressure is solidified 8 hours in 80 DEG C, obtains above-mentioned polyurethane wave-absorbing material.
Performance test
Using the identical method with being provided in embodiment 1, the absorption ripple of the polyurethane wave-absorbing material provided above-described embodiment
Performance and fire resistance are detected, and testing result is：Absorbing property is less than -42 db in 4GHz~20GHz frequency ranges,
The fire resistance of above-mentioned polyurethane wave-absorbing material reaches HF-1 levels.
Embodiment 4
The embodiment of the present invention provides a kind of polyurethane wave-absorbing material and obtained by the aggregated reaction of component of following mass parts：Polyethers is more
First 100 parts of alcohol, 50 parts of toluene di-isocyanate(TDI), 0.3 part of nano carbon sol, 17 parts of deionized water, 23 parts of methyl-phosphoric acid dimethyl ester,
8 parts of carboxyl multi-walled carbon nanotube, 30 parts of ferroso-ferric oxide, 5 parts of Firebrake ZB, 0.3 part of stannous octoate, 0.45 part of triethylene diamine,
2 parts of organic silicon surfactant, 7 parts of sodium acid carbonate.
The embodiment of the present invention also provides a kind of preparation method of above-mentioned polyurethane wave-absorbing material, the preparation method and embodiment
1 preparation method provided is essentially identical, and difference is：
Reaction foaming：Room temperature foamed time in the step is 90 minutes；
Freeze-drying：The step includes first freezing the absorbing material gel 60 hours, and cryogenic temperature solidifies for mixed solution
40 DEG C below point temperature；Then the mixed solution after freezing is further dried 72 hours in -80 DEG C of low-temp low-pressures, pressure is
0.8 kPa；Finally the dried mixed solution of low-temp low-pressure is solidified 6 hours in 90 DEG C, obtains above-mentioned polyurethane wave-absorbing material.
Performance test
Using the identical method with being provided in embodiment 1, the absorption ripple of the polyurethane wave-absorbing material provided above-described embodiment
Performance and fire resistance are detected, and testing result is：Absorbing property is less than -45 db in 4GHz~20GHz frequency ranges,
The fire resistance of above-mentioned polyurethane wave-absorbing material reaches HF-1 levels.
Embodiment 5
The embodiment of the present invention provides a kind of polyurethane wave-absorbing material, and it is obtained by the aggregated reaction of component of following mass parts：It is poly-
100 parts of ethoxylated polyhydric alcohol, 70 parts of toluene di-isocyanate(TDI), 0.5 part of nano carbon sol, 20 parts of deionized water, methyl-phosphoric acid dimethyl ester
30 parts, 10 parts of carboxyl multi-walled carbon nanotube, 40 parts of ferroso-ferric oxide, 10 parts of Firebrake ZB, 0.4 part of stannous octoate, triethylene diamine
0.6 part, 3 parts of organic silicon surfactant, 10 parts of sodium acid carbonate.
The embodiment of the present invention also provides a kind of preparation method of above-mentioned polyurethane wave-absorbing material, the preparation method and embodiment
1 preparation method provided is essentially identical, and difference is：
Reaction foaming：Room temperature foamed time in the step is 90 minutes；
Freeze-drying：The step includes first freezing the absorbing material gel 70 hours, and cryogenic temperature solidifies for mixed solution
50 DEG C below point temperature；Then the mixed solution after freezing is further dried 96 hours in -100 DEG C of low-temp low-pressures, pressure 1
kPa；Finally the dried mixed solution of low-temp low-pressure is solidified 4 hours in 100 DEG C, obtains above-mentioned polyurethane wave-absorbing material.
Performance test
Using the identical method with being provided in embodiment 1, the absorption ripple of the polyurethane wave-absorbing material provided above-described embodiment
Performance and fire resistance are detected, and testing result is：Absorbing property is less than -41 db in 4GHz~20GHz frequency ranges,
The fire resistance of above-mentioned polyurethane wave-absorbing material reaches HF-1 levels.
Finally it should be noted that：The above embodiments are merely illustrative of the technical scheme of the present invention and are not intended to be limiting thereof；To the greatest extent
The present invention is described in detail with reference to preferred embodiments for pipe, those of ordinary skills in the art should understand that：Still
The embodiment of the present invention can be modified or equivalent substitution is carried out to some technical characteristics；Without departing from this hair
The spirit of bright technical scheme, it all should cover among the claimed technical scheme scope of the present invention.
Claims (6)
1. a kind of polyurethane wave-absorbing material, it is characterised in that it is obtained by the aggregated reaction of component of following mass parts：Polyethers is more
First 100 parts of alcohol, 20~70 parts of toluene di-isocyanate(TDI), 0.01~0.5 part of nano carbon sol, 10~20 parts of deionized water, methyl
5~30 parts of dimethyl phosphate, 2~10 parts of carboxyl multi-walled carbon nanotube, 10~40 parts of ferroso-ferric oxide, 1~10 part of Firebrake ZB are pungent
Sour 0.02~0.4 part of stannous, 0.03~0.6 part of triethylene diamine, 0.2~3 part of organic silicon surfactant, sodium acid carbonate 1~
10 parts, wherein, the polyether polyol hydroxyl value is 30~60mgKOH/g, the finger of the isocyanates of the toluene di-isocyanate(TDI)
Number is 0.60~1.15.
2. polyurethane wave-absorbing material according to claim 1, it is characterised in that it is aggregated by the component of following mass parts
Reaction obtains：100 parts of PPG, 40~50 parts of toluene di-isocyanate(TDI), 0.1~0.3 part of nano carbon sol, deionized water
13~17 parts, 12~23 parts of methyl-phosphoric acid dimethyl ester, 4~8 parts of carboxyl multi-walled carbon nanotube, 20~30 parts of ferroso-ferric oxide, boron
Sour 5~6 parts of zinc, 0.08~0.3 part of stannous octoate, 0.12~0.45 part of triethylene diamine, 1~2 part of organic silicon surfactant,
5~7 parts of sodium acid carbonate.
3. a kind of preparation method of the polyurethane wave-absorbing material described in claim 1 or 2, it comprises the following steps：
Raw material mixes：PPG, methyl-phosphoric acid dimethyl ester, nano carbon sol, ferroso-ferric oxide, Firebrake ZB, octanoic acid is sub-
Tin, triethylene diamine, deionized water, organic silicon surfactant are stirred at room temperature uniformly, then handled through ultrasonic disperse
To first mixture；
Reaction foaming：First toluene di-isocyanate(TDI) is added into the first mixture and be stirred by ultrasonic 5~10 minutes, add
Carboxyl CNT and sodium acid carbonate, mould is then poured into rapidly and carries out room temperature foaming 30~90 minutes, absorbing material is obtained and coagulates
Glue；
Freeze-drying：The absorbing material gel be freeze-dried and produces the polyurethane wave-absorbing material.
4. the preparation method of polyurethane wave-absorbing material according to claim 3, it is characterised in that the step of the reaction foaming
Suddenly include：In the presence of ultrasonic agitation, first toluene di-isocyanate(TDI) is added under conditions of heating while stirring described
5~10 minutes in first mixture, carboxyl CNT and sodium acid carbonate are added；Then mould is poured into rapidly carries out room temperature hair
Bubble 30~90 minutes, obtains the absorbing material gel.
5. the preparation method of polyurethane wave-absorbing material according to claim 4, it is characterised in that in raw material mixing
In step, the ultrasonic disperse processing is carried out in a water bath.
6. the preparation method of the polyurethane wave-absorbing material according to claim 3 or 4 or 5 any one, it is characterised in that described
The step of freeze-drying, includes：First the absorbing material gel is freezed 10~70 hours, cryogenic temperature solidifies for mixed solution
5~50 DEG C below point temperature；Then the mixed solution after freezing is further dried 24~96 in -10~-100 DEG C of low-temp low-pressures
Hour, pressure is 0.1~1kPa；Finally the dried mixed solution of low-temp low-pressure is solidified 4~12 hours in 60~100 DEG C.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610840962.7A CN107857852A (en) | 2016-09-22 | 2016-09-22 | Polyurethane wave-absorbing material and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110483980A (en) * | 2019-08-30 | 2019-11-22 | 东北师范大学 | A kind of composite electromagnetic shield materials and its preparation method and application |
| CN116278518A (en) * | 2023-03-20 | 2023-06-23 | 安徽誉林新材料科技有限公司 | Puncture-proof and explosion-proof polyurethane tire and preparation method thereof |
-
2016
- 2016-09-22 CN CN201610840962.7A patent/CN107857852A/en not_active Withdrawn
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110483980A (en) * | 2019-08-30 | 2019-11-22 | 东北师范大学 | A kind of composite electromagnetic shield materials and its preparation method and application |
| CN110483980B (en) * | 2019-08-30 | 2021-05-25 | 东北师范大学 | Composite electromagnetic shielding material and preparation method and application thereof |
| CN116278518A (en) * | 2023-03-20 | 2023-06-23 | 安徽誉林新材料科技有限公司 | Puncture-proof and explosion-proof polyurethane tire and preparation method thereof |
| CN116278518B (en) * | 2023-03-20 | 2023-08-29 | 安徽誉林新材料科技有限公司 | Puncture-proof and explosion-proof polyurethane tire and preparation method thereof |
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Application publication date: 20180330 |