CN107868207A - Polyurethane barium titanate composite flame-proof absorbing material and preparation method thereof - Google Patents
Polyurethane barium titanate composite flame-proof absorbing material and preparation method thereof Download PDFInfo
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- C08G18/00—Polymeric products of isocyanates or isothiocyanates
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Abstract
The invention provides a kind of polyurethane barium titanate composite flame-proof 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, 2~8 parts of graphene oxide, 10~25 parts of barium titanate, 1~3 part of nano zine oxide, 1~3 part of nanometer tungsten 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 barium titanate composite flame-proof 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 barium titanate composite flame-proof absorbing material.
Description
Technical field
The invention belongs to technical field of function materials, and in particular to a kind of polyurethane barium titanate composite flame-proof absorbing material and
Its preparation method.
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 it is necessory to provide a kind of polyurethane barium titanate composite flame-proof absorbing material and its preparation side
Method, to solve the above problems.
The present invention provides a kind of polyurethane barium titanate composite flame-proof absorbing material, and it is aggregated by the component of following mass parts
Reaction obtains：100 parts of PPG, 20~70 parts of toluene di-isocyanate(TDI), 0.01~0.5 part of nano carbon sol, deionization
10~20 parts of water, 5~30 parts of methyl-phosphoric acid dimethyl ester, 2~8 parts of graphene oxide, 10~25 parts of barium titanate, nano zine oxide 1
~3 parts, 1~3 part of nanometer tungsten oxide, 1~10 part of Firebrake ZB, 0.02~0.4 part of stannous octoate, triethylene diamine 0.03~0.6
Part, 0.2~3 part of organic silicon surfactant, 1~10 part of sodium acid carbonate.
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 barium titanate composite flame-proof absorbing material by following mass parts the aggregated reaction of component
Obtain：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, 4~6 parts of graphene oxide, 15~20 parts of barium titanate, nano zine oxide 1.5~
2.5 parts, 1.5~2.5 parts of nanometer tungsten oxide, 5~6 parts of Firebrake ZB, 0.08~0.3 part of stannous octoate, triethylene diamine 0.12~
0.45 part, 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 barium titanate composite flame-proof absorbing material, and it includes following
Step：
Raw material mixes：By PPG, methyl-phosphoric acid dimethyl ester, nano carbon sol, barium titanate, Firebrake ZB, stannous octoate, three
Ethylene diamine, deionized water, organic silicon surfactant are stirred at room temperature uniformly, then handle to obtain for the first time through ultrasonic disperse
Mixture；
Reaction foaming：Toluene di-isocyanate(TDI), nano zine oxide and nanometer tungsten oxide are added into the first mixture and are surpassed
Sound stir 15~30 minutes, add graphene oxide and sodium acid carbonate, then pour into rapidly mould carry out room temperature foaming 30~
90 minutes, obtain absorbing material gel；
Freeze-drying：The absorbing material gel be freeze-dried and produces the polyurethane barium titanate composite flame-proof suction ripple material
Material.
Included based on the step of above-mentioned, the reaction is foamed：In the presence of ultrasonic agitation, first by toluene diisocynate
Ester, nano zine oxide and nanometer tungsten oxide are 15~30 points in the first mixture is added under conditions of heating while stirring
Clock, add graphene oxide and sodium acid carbonate；Then mould is poured into rapidly and carries out room temperature foaming 30~90 minutes, is obtained described
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 barium titanate composite flame-proof absorbing material provided by the invention uses methyl acid phosphate two
Methyl esters is combined with Firebrake ZB, is allowed to play fire-retardant synergy so that the polyurethane barium titanate composite flame-proof absorbing material
There is low cigarette, low toxicity, fire retardant, and the fire resistance of the material reaches HF-1 levels；Sodium acid carbonate and graphene oxide
React and produce bubble, while coordinate Freeze Drying Technique to remove the deionized water in the absorbing material gel so that system
Standby polyurethane barium titanate composite flame-proof absorbing material has a loose structure, larger specific surface area, in addition, nano carbon sol and
Graphene oxide has larger adsorptivity and electric conductivity, then coordinates with barium titanate, nano zine oxide and nanometer tungsten oxide so that
The polyurethane barium titanate composite flame-proof 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 graphene have preferable electric conductivity, and it is evenly dispersed in polyurethane-base
In body and good conductive network is formed, the electric property of preparation gained compound polyurethane material improves and stably, excess effusion value is low.
The present invention is combined to prepare the polyurethane barium titanate composite flame-proof using chemical foaming technology and orientation Freeze Drying Technique
Absorbing 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 barium titanate composite flame-proof absorbing material, and it is by the component of following mass parts through poly-
Reaction is closed to obtain：100 parts of PPG, 20 parts of toluene di-isocyanate(TDI), 0.02 part of nano carbon sol, 10 parts of deionized water,
5 parts of methyl-phosphoric acid dimethyl ester, 2 parts of graphene oxide, 10 parts of barium titanate, 1 part of nano zine oxide, 1 part of nanometer tungsten oxide, Firebrake ZB
1 part, 0.02 part of stannous octoate, 0.03 part of triethylene diamine, 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 barium titanate composite flame-proof absorbing material, and it is wrapped
Include following steps：
Raw material mixes：Above-mentioned mass parts, by PPG, methyl-phosphoric acid dimethyl ester, nano carbon sol, barium titanate, Firebrake ZB,
Stannous octoate, triethylene diamine, deionized water, organic silicon surfactant are stirred at room temperature uniformly, then through ultrasonic disperse
Processing obtains first mixture；
Reaction foaming：In the presence of ultrasonic agitation, first by toluene di-isocyanate(TDI), nano zine oxide and nanometer tungsten oxide on side
It is added under conditions of the stirring of heating side in the first mixture 15~30 minutes, adds graphene oxide and bicarbonate
Sodium；Then mould is poured into rapidly and carries out room temperature foaming 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 barium titanate composite flame-proof and inhales ripple material
Material.
Performance test
Absorbing property detection method：It is 3cm × 3cm that above-mentioned polyurethane barium titanate composite flame-proof absorbing material is cut into area,
Thickness is 4 mm rectangular patch sample, and the very smooth aluminium foil of layer of surface is sticked on a side surface, using digitlization
The microwave reflection rate curve of vector network analyzer (8722ET types) test above-mentioned sample in 4~20 ghz bands.It will detect,
Absorbing property is less than -39 db in 4GHz~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 barium titanate composite flame-proof absorbing material reaches HF-1 levels.
Embodiment 2
It is aggregated by the component of following mass parts that the embodiment of the present invention provides a kind of polyurethane barium titanate composite flame-proof absorbing material
Reaction obtains：100 parts of PPG, 30 parts of toluene di-isocyanate(TDI), 0.1 part of nano carbon sol, 13 parts of deionized water, methyl
12 parts of dimethyl phosphate, 4 parts of graphene oxide, 15 parts of barium titanate, 1.5 parts of nano zine oxide, 1.5 parts of nanometer tungsten oxide, boric acid
5 parts of zinc, 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 barium titanate composite flame-proof absorbing material, the system
Preparation Method and the preparation method that embodiment 1 provides are 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 barium titanate is obtained and answers
Close flame-retarding wave-absorbing material.
Performance test
Using the identical method with being provided in embodiment 1, the polyurethane barium titanate composite flame-proof that above-described embodiment provides is inhaled
The absorption ripple performance and fire resistance of wave material are detected, and testing result is：Absorbing property is in 4GHz~20GHz frequency ranges
Interior to be less than -43 db, the fire resistance of above-mentioned polyurethane barium titanate composite flame-proof absorbing material reaches HF-1 levels.
Embodiment 3
The embodiment of the present invention provides a kind of polyurethane barium titanate composite flame-proof absorbing material, and it is by the component of following mass parts through poly-
Reaction is closed to obtain：100 parts of PPG, 40 parts of toluene di-isocyanate(TDI), 0.2 part of nano carbon sol, 15 parts of deionized water, first
18 parts of base dimethyl phosphate, 5 parts of graphene oxide, 18 parts of barium titanate, 2 parts of nano zine oxide, 2 parts of nanometer tungsten oxide, Firebrake ZB 6
Part, 0.2 part of stannous octoate, 0.3 part of triethylene diamine, 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 barium titanate composite flame-proof absorbing material, the system
Preparation Method and the preparation method that embodiment 1 provides are 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, above-mentioned polyurethane barium titanate is obtained and answers
Close flame-retarding wave-absorbing material.
Performance test
Using the identical method with being provided in embodiment 1, the polyurethane barium titanate composite flame-proof that above-described embodiment provides is inhaled
The absorption ripple performance and fire resistance of wave material are detected, and testing result is：Absorbing property is in 4GHz~20GHz frequency ranges
Interior to be less than -48 db, the fire resistance of above-mentioned polyurethane barium titanate composite flame-proof absorbing material reaches HF-1 levels.
Embodiment 4
It is aggregated by the component of following mass parts that the embodiment of the present invention provides a kind of polyurethane barium titanate composite flame-proof absorbing material
Reaction obtains：100 parts of PPG, 50 parts of toluene di-isocyanate(TDI), 0.3 part of nano carbon sol, 17 parts of deionized water, methyl
23 parts of dimethyl phosphate, 6 parts of graphene oxide, 20 parts of barium titanate, 2.5 parts of nano zine oxide, 2.5 parts of nanometer tungsten oxide, boric acid
5 parts of zinc, 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 barium titanate composite flame-proof absorbing material, the system
Preparation Method and the preparation method that embodiment 1 provides are 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, above-mentioned polyurethane barium titanate is obtained and answers
Close flame-retarding wave-absorbing material.
Performance test
Using the identical method with being provided in embodiment 1, the polyurethane barium titanate composite flame-proof that above-described embodiment provides is inhaled
The absorption ripple performance and fire resistance of wave material are detected, and testing result is：Absorbing property is in 4GHz~20GHz frequency ranges
Interior to be less than -46 db, the fire resistance of above-mentioned polyurethane barium titanate composite flame-proof absorbing material reaches HF-1 levels.
Embodiment 5
The embodiment of the present invention provides a kind of polyurethane barium titanate composite flame-proof absorbing material, and it is by the component of following mass parts through poly-
Reaction is closed to obtain：100 parts of PPG, 70 parts of toluene di-isocyanate(TDI), 0.5 part of nano carbon sol, 20 parts of deionized water, first
30 parts of base dimethyl phosphate, 8 parts of graphene oxide, 25 parts of barium titanate, 3 parts of nano zine oxide, 3 parts of nanometer tungsten oxide, Firebrake ZB
10 parts, 0.4 part of stannous octoate, 0.6 part of triethylene diamine, 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 barium titanate composite flame-proof absorbing material, the system
Preparation Method and the preparation method that embodiment 1 provides are 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 the above-mentioned compound resistance of polyurethane barium titanate
Burn and suck wave material.
Performance test
Using the identical method with being provided in embodiment 1, the polyurethane barium titanate composite flame-proof that above-described embodiment provides is inhaled
The absorption ripple performance and fire resistance of wave material are detected, and testing result is：Absorbing property is in 4GHz~20GHz frequency ranges
Interior to be less than -45 db, the fire resistance of above-mentioned polyurethane barium titanate composite flame-proof 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 barium titanate composite flame-proof absorbing material, it is characterised in that it is aggregated by the component of following mass parts
Reaction obtains：100 parts of PPG, 20~70 parts of toluene di-isocyanate(TDI), 0.01~0.5 part of nano carbon sol, deionization
10~20 parts of water, 5~30 parts of methyl-phosphoric acid dimethyl ester, 2~8 parts of graphene oxide, 10~25 parts of barium titanate, nano zine oxide 1
~3 parts, 1~3 part of nanometer tungsten oxide, 1~10 part of Firebrake ZB, 0.02~0.4 part of stannous octoate, triethylene diamine 0.03~0.6
Part, 0.2~3 part of organic silicon surfactant, 1~10 part of sodium acid carbonate, wherein, the polyether polyol hydroxyl value be 30~
60mgKOH/g, the index of the isocyanates of the toluene di-isocyanate(TDI) is 0.60~1.15.
2. polyurethane barium titanate composite flame-proof absorbing material according to claim 1, it is characterised in that it is by following quality
The aggregated reaction of component of part obtains：100 parts of PPG, 40~50 parts of toluene di-isocyanate(TDI), nano carbon sol 0.1~
0.3 part, 13~17 parts of deionized water, 12~23 parts of methyl-phosphoric acid dimethyl ester, 4~6 parts of graphene oxide, barium titanate 15~20
Part, 1.5~2.5 parts of nano zine oxide, 1.5~2.5 parts of nanometer tungsten oxide, 5~6 parts of Firebrake ZB, stannous octoate 0.08~0.3
Part, 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 barium titanate composite flame-proof absorbing material described in claim 1 or 2, it includes following
Step：
Raw material mixes：By PPG, methyl-phosphoric acid dimethyl ester, nano carbon sol, barium titanate, Firebrake ZB, stannous octoate, three
Ethylene diamine, deionized water, organic silicon surfactant are stirred at room temperature uniformly, then handle to obtain for the first time through ultrasonic disperse
Mixture；
Reaction foaming：Toluene di-isocyanate(TDI), nano zine oxide and nanometer tungsten oxide are added into the first mixture and are surpassed
Sound stir 15~30 minutes, add graphene oxide and sodium acid carbonate, then pour into rapidly mould carry out room temperature foaming 30~
90 minutes, obtain absorbing material gel；
Freeze-drying：The absorbing material gel be freeze-dried and produces the polyurethane barium titanate composite flame-proof suction ripple material
Material.
4. the preparation method of polyurethane barium titanate composite flame-proof absorbing material according to claim 3, it is characterised in that institute
The step of stating reaction foaming includes：In the presence of ultrasonic agitation, first by toluene di-isocyanate(TDI), nano zine oxide and nano oxygen
Change tungsten 15~30 minutes in the first mixture is added under conditions of heating while stirring, add graphene oxide and
Sodium acid carbonate；Then mould is poured into rapidly and carries out room temperature foaming 30~90 minutes, obtains the absorbing material gel.
5. the preparation method of polyurethane barium titanate composite flame-proof absorbing material according to claim 4, it is characterised in that
In the step of raw material mixing, the ultrasonic disperse processing is carried out in a water bath.
6. the preparation method of the polyurethane barium titanate composite flame-proof absorbing material according to claim 3 or 4 or 5 any one,
Characterized in that, the step of freeze-drying, includes：First the absorbing material gel is freezed 10~70 hours, cryogenic temperature
For 5~50 DEG C below mixed solution freezing point temperature；Then by the mixed solution after freezing further in -10~-100 DEG C of low temperature
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
Solidification 4~12 hours.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610845851.5A CN107868207A (en) | 2016-09-23 | 2016-09-23 | Polyurethane barium titanate composite flame-proof absorbing material and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109503794A (en) * | 2018-11-13 | 2019-03-22 | 江苏奥斯佳材料科技股份有限公司 | A kind of polyurethane rigid foam composition and polyurethane rigid foam material and preparation method thereof |
| CN111218189A (en) * | 2018-11-26 | 2020-06-02 | 西安光启尖端技术研究院 | Resistive film and preparation method and application thereof |
-
2016
- 2016-09-23 CN CN201610845851.5A patent/CN107868207A/en not_active Withdrawn
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109503794A (en) * | 2018-11-13 | 2019-03-22 | 江苏奥斯佳材料科技股份有限公司 | A kind of polyurethane rigid foam composition and polyurethane rigid foam material and preparation method thereof |
| CN113501924A (en) * | 2018-11-13 | 2021-10-15 | 江苏奥斯佳材料科技股份有限公司 | Polyurethane rigid foam thermal insulation material |
| CN111218189A (en) * | 2018-11-26 | 2020-06-02 | 西安光启尖端技术研究院 | Resistive film and preparation method and application thereof |
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Application publication date: 20180403 |