CN107857854A - Polyurethane flame-proof inhales ripple porous material and preparation method thereof - Google Patents
Polyurethane flame-proof inhales ripple porous material and preparation method thereof Download PDFInfo
- Publication number
- CN107857854A CN107857854A CN201610843738.3A CN201610843738A CN107857854A CN 107857854 A CN107857854 A CN 107857854A CN 201610843738 A CN201610843738 A CN 201610843738A CN 107857854 A CN107857854 A CN 107857854A
- Authority
- CN
- China
- Prior art keywords
- parts
- porous material
- proof
- polyurethane flame
- inhales
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Withdrawn
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- 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
- C08G18/40—High-molecular-weight compounds
- C08G18/48—Polyethers
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
- C08J9/06—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent
- C08J9/08—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent developing carbon dioxide
-
- 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
- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
- C08K13/04—Ingredients characterised by their shape and organic or inorganic ingredients
-
- 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
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
-
- 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
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
-
- 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
- C08K3/38—Boron-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
- C08K7/00—Use of ingredients characterised by shape
- C08K7/22—Expanded, porous or hollow particles
- C08K7/24—Expanded, porous or hollow particles inorganic
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G2101/00—Manufacture of cellular products
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2203/00—Foams characterized by the expanding agent
- C08J2203/02—CO2-releasing, e.g. NaHCO3 and citric acid
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2375/00—Characterised by the use of polyureas or polyurethanes; Derivatives of such polymers
- C08J2375/04—Polyurethanes
- C08J2375/08—Polyurethanes from polyethers
-
- 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
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2265—Oxides; Hydroxides of metals of iron
- C08K2003/2275—Ferroso-ferric oxide (Fe3O4)
-
- 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
- C08K3/38—Boron-containing compounds
- C08K2003/387—Borates
-
- 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
- C08K2201/00—Specific properties of additives
- C08K2201/001—Conductive additives
-
- 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
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
Abstract
The invention provides a kind of polyurethane flame-proof to inhale ripple porous 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), 0.05~0.4 part of nano carbon sol, 0.2~0.5 part of Nano carbon white, 10~20 parts of deionized water, 5~25 parts of methyl-phosphoric acid dimethyl ester, 2~10 parts of carboxyl multi-walled carbon nanotube, 10~20 parts of ferroso-ferric oxide, 2~8 parts 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, 2~8 parts of sodium acid carbonate.Above-mentioned polyurethane flame-proof provided by the invention, which inhales ripple porous material, has the characteristics that low cigarette, low toxicity, absorption frequency distribution that is fire retardant, absorbing ripple are wide.The present invention also provides the preparation method that a kind of above-mentioned polyurethane flame-proof inhales ripple porous material.
Description
Technical field
The invention belongs to technical field of function materials, and in particular to a kind of polyurethane flame-proof inhales ripple porous 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 inhales ripple porous material and preparation method thereof it is necessory to provide a kind of polyurethane flame-proof, with
Solve the above problems.
The present invention provides a kind of polyurethane flame-proof and inhales ripple porous material, and it aggregated is reacted by the component of following mass parts
Arrive：100 parts of PPG, 20~70 parts of toluene di-isocyanate(TDI), 0.05~0.4 part of nano carbon sol, Nano carbon white 0.2
~0.5 part, 10~20 parts of deionized water, 5~25 parts of methyl-phosphoric acid dimethyl ester, 2~10 parts of carboxyl multi-walled carbon nanotube, four oxidations
10~20 parts of three-iron, 2~8 parts of Firebrake ZB, 0.02~0.4 part of stannous octoate, 0.03~0.6 part of triethylene diamine, organosilicon table
0.2~3 part of face activating agent, 2~8 parts 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 flame-proof is inhaled ripple porous material and obtained by the aggregated reaction of component of following mass parts：
100 parts of PPG, 40~50 parts of toluene di-isocyanate(TDI), 0.15~0.25 part of nano carbon sol, Nano carbon white 0.3~
0.4 part, 13~17 parts of deionized water, 10~20 parts of methyl-phosphoric acid dimethyl ester, 4~8 parts of carboxyl multi-walled carbon nanotube, four oxidations three
13~17 parts of iron, 4~6 parts of Firebrake ZB, 0.08~0.3 part of stannous octoate, 0.12~0.45 part of triethylene diamine, organosilyl surface
1~2 part of activating agent, 4~6 parts of sodium acid carbonate.
The present invention also provides the preparation method that a kind of above-mentioned polyurethane flame-proof inhales ripple porous material, and it comprises the following steps：
Raw material mixes：By PPG, methyl-phosphoric acid dimethyl ester, nano carbon sol, Nano carbon white, 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：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 flame-proof suction ripple porous 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 multi-walled carbon nanotube is added
And sodium acid carbonate；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 flame-proof provided by the invention inhale ripple porous material using methyl-phosphoric acid dimethyl ester with
Firebrake ZB is combined, and is allowed to play fire-retardant synergy so that the polyurethane flame-proof, which inhales ripple porous material, has low cigarette, low
The features such as malicious, fire retardant, and the fire resistance of the material reaches HF-1 levels；Sodium acid carbonate occurs anti-with carboxyl multi-walled carbon nanotube
Bubble should be produced, while coordinates Freeze Drying Technique to remove the deionized water in the absorbing material gel so that preparation gathers
Urethane flame-retarding wave-absorbing porous material has a loose structure, larger specific surface area, in addition, nano carbon sol, Nano carbon white and
Carboxyl multi-walled carbon nanotube has larger adsorptivity, then coordinates with ferroso-ferric oxide so that it is more that the polyurethane flame-proof inhales ripple
Porous materials have higher wave absorbing efficiency, and absorption frequency distribution is wide, suitable for wave-absorbing and camouflage field.Further, since nano-sized carbon is molten
Glue and CNT have preferable electric conductivity, and are evenly dispersed in polyurethane matrix and form good conductive mesh
Network, the electric property of preparation gained compound polyurethane material improves and stably, excess effusion value is low.The present invention uses chemical foaming technology
It is combined with orientation Freeze Drying Technique and inhales ripple porous material to prepare the polyurethane flame-proof, preparation technology is simple, small investment,
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 flame-proof and inhales ripple porous material, its by following mass parts the aggregated reaction of component
Obtain：100 parts of PPG, 20 parts of toluene di-isocyanate(TDI), 0.05 part of nano carbon sol, 0.2 part of Nano carbon white, go from
Sub- 10 parts of water, 5 parts of methyl-phosphoric acid dimethyl ester, 2 parts of carboxyl multi-walled carbon nanotube, 10 parts of ferroso-ferric oxide, 2 parts of Firebrake ZB, octanoic acid
0.02 part of stannous, 0.03 part of triethylene diamine, 0.2 part of organic silicon surfactant, 2 parts of sodium acid carbonate.
The embodiment of the present invention also provides the preparation method that a kind of above-mentioned polyurethane flame-proof inhales ripple porous material, and it includes following
Step：
Raw material mixes：Above-mentioned mass parts, by PPG, methyl-phosphoric acid dimethyl ester, nano carbon sol, Nano carbon white, four
Fe 3 O, Firebrake ZB, stannous octoate, triethylene diamine, deionized water, organic silicon surfactant are stirred at room temperature
It is even, then handle to obtain first mixture through ultrasonic disperse；
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 multi-walled carbon nanotube and sodium acid carbonate are added；Then mould is poured into rapidly
Carry out room temperature to foam 30 minutes, obtain 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 flame-proof and inhales ripple porous material.
Performance test
Absorbing property detection method：It is 3cm × 3cm that above-mentioned polyurethane flame-proof suction ripple porous material is cut into area, thickness 4
Mm rectangular patch sample, and the very smooth aluminium foil of layer of surface is sticked on a side surface, using digital vector network
The microwave reflection rate curve of analyzer (8722ET types) test above-mentioned sample in 4~20 ghz bands.It will detect, absorbing property
It is less than -34 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 flame-proof suction ripple porous material reaches HF-1 levels.
Embodiment 2
The embodiment of the present invention, which provides a kind of polyurethane flame-proof, inhales ripple porous material and aggregated is reacted by the component of following mass parts
Arrive：100 parts of PPG, 30 parts of toluene di-isocyanate(TDI), 0.15 part of nano carbon sol, 0.3 part of Nano carbon white, deionization
13 parts of water, 10 parts of methyl-phosphoric acid dimethyl ester, 4 parts of carboxyl multi-walled carbon nanotube, 13 parts of ferroso-ferric oxide, 4 parts of Firebrake ZB, octanoic acid are sub-
0.08 part of tin, 0.12 part of triethylene diamine, 1 part of organic silicon surfactant, 4 parts of sodium acid carbonate.
The embodiment of the present invention also provides the preparation method that a kind of above-mentioned polyurethane flame-proof inhales ripple porous material, the preparation method
The preparation method provided with embodiment 1 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 flame-proof is obtained and inhales ripple
Porous material.
Performance test
Using the identical method with being provided in embodiment 1, ripple porous material is inhaled to the polyurethane flame-proof that above-described embodiment provides
Absorption ripple performance and fire resistance detected, testing result is：Absorbing property is small in 4GHz~20GHz frequency ranges
In -37 db, the fire resistance that above-mentioned polyurethane flame-proof inhales ripple porous material reaches HF-1 levels.
Embodiment 3
The embodiment of the present invention provides a kind of polyurethane flame-proof and inhales ripple porous material, its by following mass parts the aggregated reaction of component
Obtain：100 parts of PPG, 40 parts of toluene di-isocyanate(TDI), 0.2 part of nano carbon sol, 0.35 part of Nano carbon white, go from
Sub- 15 parts of water, 15 parts of methyl-phosphoric acid dimethyl ester, 6 parts of carboxyl multi-walled carbon nanotube, 15 parts of ferroso-ferric oxide, 5 parts of Firebrake ZB, octanoic acid
0.2 part of stannous, 0.3 part of triethylene diamine, 1.6 parts of organic silicon surfactant, 5 parts of sodium acid carbonate.
The embodiment of the present invention also provides the preparation method that a kind of above-mentioned polyurethane flame-proof inhales ripple porous material, the preparation method
The preparation method provided with embodiment 1 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, above-mentioned polyurethane flame-proof is obtained and inhales ripple
Porous material.
Performance test
Using the identical method with being provided in embodiment 1, ripple porous material is inhaled to the polyurethane flame-proof that above-described embodiment provides
Absorption ripple performance and fire resistance detected, testing result is：Absorbing property is small in 4GHz~20GHz frequency ranges
In -40 db, the fire resistance that above-mentioned polyurethane flame-proof inhales ripple porous material reaches HF-1 levels.
Embodiment 4
The embodiment of the present invention, which provides a kind of polyurethane flame-proof, inhales ripple porous material and aggregated is reacted by the component of following mass parts
Arrive：100 parts of PPG, 50 parts of toluene di-isocyanate(TDI), 0.25 part of nano carbon sol, 0.4 part of Nano carbon white, deionization
17 parts of water, 20 parts of methyl-phosphoric acid dimethyl ester, 8 parts of carboxyl multi-walled carbon nanotube, 17 parts of ferroso-ferric oxide, 6 parts of Firebrake ZB, octanoic acid are sub-
0.3 part of tin, 0.45 part of triethylene diamine, 2 parts of organic silicon surfactant, 6 parts of sodium acid carbonate.
The embodiment of the present invention also provides the preparation method that a kind of above-mentioned polyurethane flame-proof inhales ripple porous material, the preparation method
The preparation method provided with embodiment 1 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, above-mentioned polyurethane flame-proof is obtained and inhales ripple
Porous material.
Performance test
Using the identical method with being provided in embodiment 1, ripple porous material is inhaled to the polyurethane flame-proof that above-described embodiment provides
Absorption ripple performance and fire resistance detected, testing result is：Absorbing property is small in 4GHz~20GHz frequency ranges
In -42 db, the fire resistance that above-mentioned polyurethane flame-proof inhales ripple porous material reaches HF-1 levels.
Embodiment 5
The embodiment of the present invention provides a kind of polyurethane flame-proof and inhales ripple porous material, its by following mass parts the aggregated reaction of component
Obtain：100 parts of PPG, 70 parts of toluene di-isocyanate(TDI), 0.4 part of nano carbon sol, 0.5 part of Nano carbon white, go from
Sub- 20 parts of water, 25 parts of methyl-phosphoric acid dimethyl ester, 10 parts of carboxyl multi-walled carbon nanotube, 20 parts of ferroso-ferric oxide, 8 parts of Firebrake ZB are pungent
Sour 0.4 part of stannous, 0.6 part of triethylene diamine, 3 parts of organic silicon surfactant, 8 parts of sodium acid carbonate.
The embodiment of the present invention also provides the preparation method that a kind of above-mentioned polyurethane flame-proof inhales ripple porous material, the preparation method
The preparation method provided with embodiment 1 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, it is porous to obtain above-mentioned polyurethane flame-proof suction ripple
Material.
Performance test
Using the identical method with being provided in embodiment 1, ripple porous material is inhaled to the polyurethane flame-proof that above-described embodiment provides
Absorption ripple performance and fire resistance detected, testing result is：Absorbing property is small in 4GHz~20GHz frequency ranges
In -41 db, the fire resistance that above-mentioned polyurethane flame-proof inhales ripple porous 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 flame-proof inhales ripple porous material, it is characterised in that it aggregated is reacted by the component of following mass parts
Arrive：100 parts of PPG, 20~70 parts of toluene di-isocyanate(TDI), 0.05~0.4 part of nano carbon sol, Nano carbon white 0.2
~0.5 part, 10~20 parts of deionized water, 5~25 parts of methyl-phosphoric acid dimethyl ester, 2~10 parts of carboxyl multi-walled carbon nanotube, four oxidations
10~20 parts of three-iron, 2~8 parts of Firebrake ZB, 0.02~0.4 part of stannous octoate, 0.03~0.6 part of triethylene diamine, organosilicon table
0.2~3 part of face activating agent, 2~8 parts of sodium acid carbonate, wherein, the polyether polyol hydroxyl value is 30~60mgKOH/g, the first
The index of the isocyanates of phenylene diisocyanate is 0.60~1.15.
2. polyurethane flame-proof according to claim 1 inhales ripple porous material, it is characterised in that it by following mass parts group
Lease making polymerisation obtains：100 parts of PPG, 40~50 parts of toluene di-isocyanate(TDI), nano carbon sol 0.15~0.25
Part, 0.3~0.4 part of Nano carbon white, 13~17 parts of deionized water, 10~20 parts of methyl-phosphoric acid dimethyl ester, the more wall carbon of carboxyl are received
4~8 parts of mitron, 13~17 parts of ferroso-ferric oxide, 4~6 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, 4~6 parts of sodium acid carbonate.
3. the polyurethane flame-proof described in a kind of claim 1 or 2 inhales the preparation method of ripple porous material, it comprises the following steps：
Raw material mixes：By PPG, methyl-phosphoric acid dimethyl ester, nano carbon sol, Nano carbon white, 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：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 flame-proof suction ripple porous material.
4. polyurethane flame-proof according to claim 3 inhales the preparation method of ripple porous material, it is characterised in that the reaction
The step of foaming, includes：In the presence of ultrasonic agitation, first toluene di-isocyanate(TDI) is added under conditions of heating while stirring
Enter into the first mixture 5~10 minutes, add carboxyl multi-walled carbon nanotube and sodium acid carbonate；Then mould is poured into rapidly
Tool carries out room temperature and foamed 30~90 minutes, obtains the absorbing material gel.
5. polyurethane flame-proof according to claim 4 inhales the preparation method of ripple porous material, it is characterised in that in the original
In the step of material mixing, the ultrasonic disperse processing is carried out in a water bath.
6. the polyurethane flame-proof according to claim 3 or 4 or 5 any one inhales the preparation method of ripple porous material, its feature
It is, includes the step of the freeze-drying：First the absorbing material gel is freezed 10~70 hours, cryogenic temperature is mixing
5~50 DEG C below solution freezing point temperature；Then the mixed solution after freezing is further done in -10~-100 DEG C of low-temp low-pressures
Dry 24~96 hours, pressure was 0.1~1kPa；Finally by the dried mixed solution of low-temp low-pressure in 60~100 DEG C solidify 4~
12 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610843738.3A CN107857854A (en) | 2016-09-22 | 2016-09-22 | Polyurethane flame-proof inhales ripple porous material and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610843738.3A CN107857854A (en) | 2016-09-22 | 2016-09-22 | Polyurethane flame-proof inhales ripple porous material and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107857854A true CN107857854A (en) | 2018-03-30 |
Family
ID=61699023
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610843738.3A Withdrawn CN107857854A (en) | 2016-09-22 | 2016-09-22 | Polyurethane flame-proof inhales ripple porous material and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107857854A (en) |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0600387A1 (en) * | 1992-11-30 | 1994-06-08 | Mitsubishi Cable Industries, Ltd. | Wideband wave absorber |
| CN103172828A (en) * | 2013-04-02 | 2013-06-26 | 江苏瑞丰科技实业有限公司 | Preparation of polyurethane wave-absorbing gel material |
-
2016
- 2016-09-22 CN CN201610843738.3A patent/CN107857854A/en not_active Withdrawn
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0600387A1 (en) * | 1992-11-30 | 1994-06-08 | Mitsubishi Cable Industries, Ltd. | Wideband wave absorber |
| CN103172828A (en) * | 2013-04-02 | 2013-06-26 | 江苏瑞丰科技实业有限公司 | Preparation of polyurethane wave-absorbing gel material |
Non-Patent Citations (2)
| Title |
|---|
| 刘玉荣: "《碳材料在超级电容器中的应用》", 31 January 2013, 国防工业出版社 * |
| 夏德贵: "《软磁铁氧体制造原理与技术》", 31 December 2010, 陕西科学技术出版社 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103172828A (en) | Preparation of polyurethane wave-absorbing gel material | |
| CN103408788B (en) | Flame-retardance wave-absorbing polystyrene foam material and preparation method thereof | |
| CN109664566B (en) | Light broadband wave-absorbing composite material with multilayer structure and preparation method thereof | |
| CN103087347B (en) | Polyimide composite wave absorbing foam material and preparation method thereof | |
| CN102977587A (en) | Foaming type polyurethane wave-absorbing material and preparation method thereof | |
| CN107857850A (en) | Polyurethane inhales wave resistance combustible material and preparation method thereof | |
| CN108795379A (en) | A kind of preparation method of three-dimensional netted multi-walled carbon nanotube/Ni ferrite composite wave-suction material | |
| CN106340726A (en) | Magnetic conductive nano-metal/carbon airgel absorbing material and the preparation method thereof | |
| CN103887033A (en) | Method for preparing activated carbon capable of absorbing electromagnetic waves | |
| CN107857857A (en) | Polyurethane composite wave-absorbing porous material and preparation method thereof | |
| CN107857852A (en) | Polyurethane wave-absorbing material and preparation method thereof | |
| CN107868207A (en) | Polyurethane barium titanate composite flame-proof absorbing material and preparation method thereof | |
| CN107868220A (en) | Polyurethane ferrite composite wave-suction material and preparation method thereof | |
| CN107868221A (en) | Polyurethane barium titanate composite wave-absorbing porous material and preparation method thereof | |
| CN110862671B (en) | Metal organic framework material/polyurethane wave-absorbing material and preparation method thereof | |
| CN105585725A (en) | Preparation method and application of heat insulating and inflaming retarding foam material and | |
| CN107857851A (en) | Polyurethane composite flame-retardant inhales ripple porous material and preparation method thereof | |
| CN107857987A (en) | Polyurethane composite flame-retardant absorbing material and preparation method thereof | |
| CN107857853A (en) | Polyurethane inhales wave resistance combustion porous material and preparation method thereof | |
| CN110054182A (en) | A kind of magnetic graphite alkenyl inhales wave cellular material and preparation method thereof | |
| CN107857854A (en) | Polyurethane flame-proof inhales ripple porous material and preparation method thereof | |
| CN107857863A (en) | Polyurethane inhales ripple porous material and preparation method thereof | |
| CN107857849A (en) | Polyurethane flame-proof absorbing material and preparation method thereof | |
| CN107868222A (en) | Polyurethane ferrite composite flame-proof absorbing material and preparation method thereof | |
| CN107868213A (en) | Polyurethane barium titanate composite flame-proof inhales ripple porous material and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WW01 | Invention patent application withdrawn after publication | ||
| WW01 | Invention patent application withdrawn after publication |
Application publication date: 20180330 |