CN108948409A - A kind of sound absorption Polyimide foams and preparation method thereof - Google Patents
A kind of sound absorption Polyimide foams and preparation method thereof Download PDFInfo
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- CN108948409A CN108948409A CN201810599894.9A CN201810599894A CN108948409A CN 108948409 A CN108948409 A CN 108948409A CN 201810599894 A CN201810599894 A CN 201810599894A CN 108948409 A CN108948409 A CN 108948409A
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- 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
- C08J9/12—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 physical blowing agent
- C08J9/14—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 physical blowing agent organic
- C08J9/142—Compounds containing oxygen but no halogen atom
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- 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
- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/06—Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
- C08G73/10—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
- C08G73/1003—Preparatory processes
- C08G73/1035—Preparatory processes from tetracarboxylic acids or derivatives and diisocyanates
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- 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
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- 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
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- 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
- C08J2203/12—Organic compounds only containing carbon, hydrogen and oxygen atoms, e.g. ketone or alcohol
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- 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
- C08J2379/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen, or carbon only, not provided for in groups C08J2361/00 - C08J2377/00
- C08J2379/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
- C08J2379/08—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
Abstract
The present invention provides a kind of sound absorption Polyimide foams and preparation method thereof, comprising the following steps: pours into isocyanates in A batch can；Aromatic dianhydride is dissolved into solvent and is cooled down, and foaming agent and foam stabilizer are added in the solution, is poured into B tank after mixing evenly；Sound-absorbing material and catalyst are poured into after mixing evenly in C tank；A, B, C tank are stirred respectively, through the air in multiple vacuum nitrogen gas removal raw material, is foamed by being injected into mold after closed mixing chamber mixed at high speed, then carries out microwave treatment；It is finally heat-treated in an oven, mold is removed after baking can prepare the Polyimide foams.The present invention adds a variety of sound-absorbing materials, and at low cost, preparation process is relatively simple, and sound absorption Polyimide foams are prepared by one-step method, the efficient heat insulation and acoustic absorption flame-retarding characteristic of the material can be assigned, it can be achieved that material lightweight, with good application prospect.
Description
Technical field
The present invention relates to new material technology field more particularly to a kind of sound absorption Polyimide foams and its preparation sides
Method.
Background technique
Polyimide foam is applied relatively broad in the heat-insulated field that absorbs sound at present, is mainly used in aerospace, traffic fortune
The high-tech areas such as defeated, electronics.Common sound-absorbing material such as perforation or closed pore is inorganic larger with metal material density, common to absorb sound
Foamed material temperature tolerance is lower and the pernicious gas generated that burns is easy to generate harm to human body and natural environment.And polyimides
Foam density is lower, is resistant to 200 degree of high temperature, has outstanding sound absorption flame retardant property, it is thermal insulation and sound-absorbing material that construction is simple is convenient
The outstanding selection in field.
Chinese patent CN201010144568.2 discloses a kind of polyimide foam and preparation method thereof.This method
It reacts to obtain polyimide foam precursor solution with isocyanates for aromatic dianhydride or aromatic series tetracid, foaming agent is added to
It is reacted in foam precursors solution, free foaming forms foam intermediate, solidifies foam intermediate by heat treatment.This method is
Hard polyimide foaming is prepared, sound-absorbing material, density>65kg/m3, average sound absorption coefficient<0.46 are not added with.Its density and suction
Audio fruit is all ideal not to the utmost.
Chinese patent CN201310027793.1 discloses a kind of polyimides composite wave-absorbing foamed material and its preparation side
Method.This method through foamable obtains the polyimide microsphere of part imidizate after needing to crush presoma, then again will
The polyimide microsphere is dipped into the dispersion liquid being made of wave absorbing agent and organic solvent, finally that the polyamides of soaking mistake is sub-
Amine microballoon carries out hot pressing and obtains the polyimides composite wave-absorbing foamed material.It uses powder foam method, and more together
Soaking cycle, technique is more complex, and production efficiency is lower.
Chinese patent CN201310172349.9 discloses a kind of Polyimide foam composite material.This method is using inorganic
Material glass bead and graphene film are prepared for the heat insulation and acoustic absorption Polyimide foam composite material that density is 20-50g/cm3.
Similar Chinese patent CN201410333015.X disclose a kind of hollow beads enhance polyimide-based composite foam material and
Preparation method uses hollow glass microbead to be prepared for density as 23-35g/cm3, and average sound absorption coefficient is 0.40~0.51
Absorb sound polyimide-based composite foam material.In addition, Chinese patent CN201510880307.X, which discloses one kind, has filling function
Can filler preparation method, aromatic dianhydride and aromatic diamines carry out esterification by this method, using hollow glass microbead, hollow
Ceramic microbead, expanded vermiculite or porous mineral powder prepare polyimides composite foam material by liquid phase method foam process.It is above-mentioned
Three patents all use inorganic material as sound-absorbing material, and inorganic material is easy sedimentation or layering in foaming system, compatible
Property and uniformity it is poor, be difficult to prepare reliable in quality and stable polyimide foam product.
Summary of the invention
To overcome preparation process existing in the prior art complicated, the problems such as the inorganic sound-absorbing material poor compatibility of addition,
The present invention provides a kind of sound absorption Polyimide foams and preparation method thereof.
Above-mentioned purpose that the invention is realized by the following technical scheme: a kind of sound absorption Polyimide foams, raw material include
Aromatic dianhydride, isocyanates, surfactant, foaming agent, catalyst, sound-absorbing material, the Material Percentage are as follows: isocyanic acid
Ester mass fraction 10%~62%, aromatic dianhydride mass fraction 15%~65%, solvent quality number 15%~35%, foaming
Agent mass fraction 5%~18%, foam stabilizer mass fraction 1%~9%, catalyst quality number 0.2%~7%, sound-absorbing material
Mass fraction 1%~9%.
On this basis, the middle isocyanates is aromatic isocyanate, aliphatic isocyanates and aromatic ester race isocyanide
One or more of acid esters.
On this basis, the middle aromatic dianhydride is pyromellitic acid anhydride, 3,3 ' 4,4 '-benzophenone tetracarboxylics two
Acid anhydride, 3,3 ' 4,4 '-diphenyl thio-ether tetrformate dianhydrides, 4 ' 4- diphenyl ether dianhydrides, 2,3,3 ', 4 '-diphenyl ether tetraformic dianhydrides, 3,3 '
One or more of 4,4 '-biphenyl dianhydrides and 3,3 ' 4,4 '-triphen bis ether tetracarboxylic acid dianhydrides.
On this basis, the solvent is ethyl alcohol, dimethyl sulfoxide, N ' N-dimethylformamide, N ' N dimethyl acetamide
One or more of.
On this basis, the foaming agent is acetone, tetrahydrofuran, water, methanol, ethyl alcohol, butyl glycol ether, diethylene glycol
One or more of butyl oxide, ethylene glycol -600；
On this basis, the foam stabilizer is polyether modified siloxane, polyether modified silicon oil, silicone, silicone ethylene glycol
The one or more of copolymer, organic silicon polyether copolymer surfactants, water-soluble silicon oil；
On this basis, the middle catalyst is one or more of amines catalyst or metallic catalyst.
On this basis, organic sound-absorbing material includes polymer micro mist, organosilicon microballoon, organic porous material and plant
One of object organic fiber porous material is a variety of.
On this basis, a kind of preparation method for the Polyimide foams that absorb sound, comprising the following steps:
Step 1: isocyanates is poured into A batch can；
Step 2: aromatic dianhydride is dissolved into solvent and is cooled down；
Step 3: foaming agent and foam stabilizer are added in solution made from step 2, poured into B tank after mixing evenly；
Step 4: sound-absorbing material and catalyst are poured into after mixing evenly in C tank；
Step 5: A, B, C tank are stirred respectively, by the air in vacuum nitrogen gas removal raw material；
Step 6: by the flow of computer control A, B, C batch can, by being injected into mould after the completion of closed mixing chamber mixed at high speed
It foams in tool, then carries out microwave treatment；
Step 7: being finally heat-treated in an oven, and mold is removed after the completion of baking can prepare the polyamides
Imine foam material.
On this basis, solution temperature is 95-125 DEG C in the step 2, and being cooled to temperature is 25-55 DEG C.
On this basis, in the step 5 A batch can speed of agitator be 10~2500rpm, B batch can speed of agitator be 10~
2500rpm, C batch can speed of agitator are 10~4000rpm, and mixing chamber revolving speed is 1000~4300rpm.
On this basis, microwave per kilogram processing power is 0.15~0.45kW in the step 6.
On this basis, oven temperature is 160~245 DEG C in the step 7.
Compared with prior art, the beneficial effects of the present invention are: a kind of sound absorption polyimide foam material provided by the invention
Material and preparation method thereof, only with organic sound-absorbing material, can mix in system and be uniformly dispersed, can not only simplify production work
Skill can effectively adjust the density of composite material, the machinery such as acoustic absorptivity and Compression and Expansion by changing the content of component
Performance, thus the application under meeting different condition.The abrasion for adding inorganic sound-absorbing material to the special gear of equipment is avoided simultaneously
And it blocks conveyance conduit or the problems such as tube wall remains, is conducive to the production and maintenance of pipeline and equipment.The present invention adopts
Each raw material proportioning is accurately controlled with computer-controlled closed injector, and is mixed in airtight cavity, with routine in air
The Polyimide foams of mechanical stirring mixed phase ratio, preparation have finer and smoother foam structure.Preparation of the invention simultaneously
Method the degree of automation is higher, is suitble to industrialized production.Foamed material obtained by the present invention has cell size distribution uniform
And the fine and smooth, ultralow (10kg/m of density3Left and right), heat resistance, mechanical property and sound absorbing performance it is excellent (average sound absorption coefficient >=
0.60) the features such as.It can satisfy ships and light boats and rail traffic loss of weight, sound-absorption and heat-insulation, high/low temperature heat preservation, insulation fire prevention and ventilation steamed
The fields such as steam pipe road use the requirement of Polyimide foams.
Detailed description of the invention
Fig. 1 is the average noise reduction coefficient curve graph of Polyimide foams prepared by the embodiment of the present invention 2；
Fig. 2 is the aperture figure of Polyimide foams prepared by the embodiment of the present invention 2；
Fig. 3 is the average noise reduction coefficient curve graph of Polyimide foams prepared by comparative example 1 of the present invention；
Fig. 4 is the aperture figure of Polyimide foams prepared by comparative example 1 of the present invention.
Specific embodiment
With reference to embodiments, the present invention will be described in further detail.It should be appreciated that specific reality described herein
Example is applied only to explain the present invention, is not intended to limit the present invention.
A kind of sound absorption Polyimide foams, raw material include aromatic dianhydride, isocyanates, surfactant, foaming
Agent, catalyst, sound-absorbing material, the Material Percentage are as follows: isocyanate number 10%~62%, aromatic dianhydride quality
Number 15%~65%, solvent quality number 15%~35%, foaming agent mass fraction 5%~18%, foam stabilizer mass fraction
1%~9%, catalyst quality number 0.2%~7%, sound-absorbing material mass fraction 1%~9%.
As the preferred embodiment of the present invention, the middle isocyanates is aromatic isocyanate, aliphatic isocyanic acid
One or more of ester and aromatic ester race isocyanates.
As the preferred embodiment of the present invention, the middle aromatic dianhydride be pyromellitic acid anhydride, 3,3 ' 4,4 '-two
Benzophenone tetracarboxylic acid dianhydride, 3,3 ' 4,4 '-diphenyl thio-ether tetrformate dianhydrides, 4 ' 4- diphenyl ether dianhydrides, 2,3,3 ', 4 '-diphenyl ether four
One or more of formic acid dianhydride, 3,3 ' 4,4 '-biphenyl dianhydrides and 3,3 ' 4,4 '-triphen bis ether tetracarboxylic acid dianhydrides；Solvent is
One or more of ethyl alcohol, dimethyl sulfoxide, N ' N-dimethylformamide, N ' N dimethyl acetamide.
As the preferred embodiment of the present invention, the foam stabilizer is polyether modified siloxane, polyether modified silicon oil, silicone
The one or more of class, silicone glycol copolymer, organic silicon polyether copolymer surfactants, water-soluble silicon oil.Such as it is empty
DC5000, DC6154, DC198, DC5143 etc. of gasification chemical product Co., Ltd；B8433, B8487 of win wound industrial group,
B8513 etc.；DC193, DC5598 etc. of Daukangnin GmbH；Momentive companyDeng.
As the preferred embodiment of the present invention, the catalyst be one of metallic catalyst, amines catalyst or
It is several.For example, amines catalyst hasAnd air chemical products Co., LtdDeng the amines catalyst of Momentive companyDeng；The free gasification work of metallic catalyst
Products Co., LtdDeng.
As the preferred embodiment of the present invention, the sound-absorbing material includes polymethyl methacrylate powder, organosilicon rubber
Glue micro mist, organosilicon hollow microsphere, poly lactide-glycolide acid microballoon, piperazine Quito pore polymer, porous aromatic skeleton are poly-
Close one of object, luffa and lotus leaf stem or a variety of.
A kind of preparation method for the Polyimide foams that absorb sound, comprising the following steps:
Step 1: isocyanates is poured into A batch can；
Step 2: aromatic dianhydride is dissolved into solvent and is cooled down；
Step 3: foaming agent and foam stabilizer are added in solution made from step 2, poured into B tank after mixing evenly；
Step 4: sound-absorbing material and catalyst are poured into after mixing evenly in C tank；
Step 5: A, B, C tank are stirred respectively, replace the air in removal raw material by vacuum nitrogen gas；
Step 6: by the flow of computer control A, B, C batch can, by being injected into mould after the completion of closed mixing chamber mixed at high speed
It foams in tool, then carries out microwave treatment；
Step 7: being finally heat-treated in an oven, and mold is removed after the completion of baking can prepare the polyamides
Imine foam material.
As the preferred embodiment of the present invention, solution temperature is 95-125 DEG C in the step 2, and being cooled to temperature is
25-55℃。
As the preferred embodiment of the present invention, A batch can speed of agitator is 10~2500rpm, B batch can in the step 5
Speed of agitator is 10~2500rpm, and C batch can speed of agitator is 10~4000rpm, and mixing chamber revolving speed is 1000~4300rpm.
As the preferred embodiment of the present invention, in the step 6 microwave per kilogram processing power be 0.15~
0.45kW。
As the preferred embodiment of the present invention, oven temperature is 160~245 DEG C in the step 7.
Embodiment 1
According to formula isocyanates 10wt%, aromatic dianhydride 65wt%, solvent 15wt%, foaming agent 5wt%, foam stabilizer
1wt%, catalyst 1wt%, sound-absorbing material 3wt% prepare Polyimide foams.Specially take the more methylenes of phenyl more than 10 parts
Quito isocyanates (PAPI) pours into A batch can.Take 35 parts of 3,3', 4,4'- biphenyl dianhydride, 5 parts of 3,3', 4,4'- diphenyl sulfide
Tetracarboxylic acid dianhydride and 25 parts of 4,4'- diphenyl ether dianhydrides, are added in 15 parts of dimethyl sulfoxides, and it is complete to be stirred to solid at 105 DEG C
Fully dissolved.2 parts of ethyl alcohol, 3 parts of N-Methyl pyrrolidone butyl ether, 0.5 part B8487 and 0.5 part are added after system is cooled to 25 DEG CIt is poured into B batch can after mixing evenly.Take 0.4 part of catalystPart catalystWith 3 parts of piperazine Quito pore polymers, poured into C batch can after mixing evenly.Set A batch can speed of agitator as
500rpm, B batch can speed of agitator are 500rpm, and C batch can speed of agitator is 1000rpm, and then A, B, C batch can are stirring respectively
While nitrogen is respectively vacuumized and being led to, the air in circulation 6 times or more removal raw materials, last nitrogen pressurization 0.05MPa~
0.1MPa is spare.The respective flow of A, B, C batch can is accurately controlled using computer-controlled closed injector, three kinds of raw materials is made to exist
Revolving speed is the mixing chamber mixed at high speed 10s of 3000rpm, is then poured into open fixed dimension mold and foams.After 10min when
When foam surface is hardened, mold is driven into large-scale microwave oven by guide rail, sets power 0.15kW, runs 10min.Then mould
Tool vehicle continues through guide rail and drives into large-scale heated oven, 245 DEG C of set temperature, toasts 3h.Last mould vehicle is transported to disassembly
Point, removing mold can be taken off prepared Polyimide foams.
Embodiment 2
According to formula isocyanates 62wt%, aromatic dianhydride 15wt%, solvent 15wt%, foaming agent 5wt%, foam stabilizer
1.8wt%, catalyst 0.2wt%, sound-absorbing material 1wt% prepare Polyimide foams.Specially take 32 parts of different Fu Er ketone
Diisocyanate (IPDI), 20 parts of hexamethylene diisocyanates (HDI) and 10 parts of modified MDI are poured into A batch can.15 part 3 is taken,
3', 4,4'- benzophenone tetracarboxylic dianhydride (BTDA)s are added in 15 parts of N-Methyl pyrrolidones, and it is completely molten to be stirred to solid at 125 DEG C
Solution.After system is cooled to 40 DEG C be added 1 part of ethyl alcohol, 2 parts of N-Methyl pyrrolidones -600,2 parts of acetone, 0.6 part of DC5000 and
1.2 parts of DC198, are poured into after mixing evenly in B batch can.Take 0.2 part of catalystIt is hollow micro- with 1 part of organosilicon
Ball is poured into after mixing evenly in C batch can.A batch can speed of agitator is set as 2500rpm, B batch can speed of agitator is 2500rpm, C
Batch can speed of agitator is 100rpm, and then A, B, C batch can are respectively vacuumized and led to nitrogen while stirring respectively, is recycled
Air in 6 times or more removal raw materials, last nitrogen pressurization 0.05MPa~0.1MPa are spare.Using computer-controlled closed
Injector accurately controls the respective flow of A, B, C batch can, makes three kinds of raw materials in the mixing chamber mixed at high speed of revolving speed 1000rpm
20s is then poured into open fixed dimension mould vehicle and foams.After 15min when foam surface is hardened, mould vehicle is by leading
Rail drives into large-scale microwave oven, sets power 0.25kW, runs 10min.Then mould vehicle continues through guide rail and drives into large size
In heated oven, 230 DEG C of set temperature, 5h is toasted.Last mould vehicle is transported to detachment point, and dismounting mold can be taken off prepared
Polyimide foams.
Embodiment 3
According to formula isocyanates 12wt%, aromatic dianhydride 17wt%, solvent 35wt%, foaming agent 18wt%, even bubble
Agent 9wt%, catalyst 7wt%, sound-absorbing material 2wt% prepare Polyimide foams.Specially take 10 parts of diphenyl methanes
Diisocyanate (MDI) and 2 parts of benzene dimethylene diisocyanate (XDI) are poured into A batch can.Take 10 parts of pyromellitic acid anhydrides
With 7 parts of 4,4'- (hexafluoro isopropyl alkene) two anhydride phthalic acids, it is added to the mixed of 10 parts of n,N-Dimethylformamide and 25 parts of dimethyl sulfoxides
It closes in solution, is stirred to solid at 95 DEG C and is completely dissolved.5 parts of methanol, 10 parts of N- methyl are added after system is cooled to 55 DEG C
Pyrrolidones butyl ether, 3 parts of tetrahydrofurans, 4 parts of DC5598,2 partsWith 3 parts of B8433, B material is poured into after mixing evenly
In tank.Take 2 parts of catalystPart catalyst2 parts of catalystWith 2
Part polymethyl methacrylate powder, is poured into after mixing evenly in C batch can.A batch can speed of agitator is set as 10rpm, B batch can stirs
Revolving speed is 10rpm, and C batch can speed of agitator is 4000rpm, and then A, B, C batch can respectively carry out taking out while stirring respectively true
Empty and logical nitrogen, circulation 6 times or more the air removed in raw materials, last nitrogen pressurization 0.05MPa~0.1MPa are spare.Using electricity
The closed injector of brain control accurately controls the respective flow of A, B, C batch can, makes three kinds of raw materials in the mixed of revolving speed 4300rpm
Chamber mixed at high speed 10s is closed, is then poured into open fixed dimension mould vehicle and foams.After 10min when foam surface is hardened,
Mould vehicle is driven into large-scale microwave oven by guide rail, sets power 0.45kW, runs 5min.Then mould vehicle, which continues through, leads
Rail drives into large-scale heated oven, 160 DEG C of set temperature, toasts 8h.Last mould vehicle is transported to detachment point, and mold is removed
Take out prepared Polyimide foams.
Embodiment 4
According to formula isocyanates 40wt%, aromatic dianhydride 25wt%, solvent 16wt%, foaming agent 9wt%, foam stabilizer
3wt%, catalyst 2wt%, sound-absorbing material 5wt% prepare Polyimide foams.Specially take 15 parts of methyl diisocyanates
Ester (TDI) and 25 parts of polyphenyl polymethylene polyisocyanates (PAPI) are poured into A batch can.Take 15 parts of 2,3,3', 4'- diphenyl ether
Tetracarboxylic acid dianhydride and 10 part 3,3', 4,4'- triphen bis ether tetracarboxylic acid dianhydrides are added to 6 parts of n,N-Dimethylformamide and 10 parts
In the mixed solution of N-Methyl pyrrolidone, solid is stirred at 115 DEG C and is completely dissolved.It is added after system is cooled to 30 DEG C
6 parts of methanol, 3 part of two N-Methyl pyrrolidone butyl oxide, 3 parts of DC5143, are poured into after mixing evenly in B batch can.Take 1 part of catalyst1 part of catalyst2 parts of porous aromatic skeleton polymer and 3 portions of luffas, after mixing evenly
It pours into C batch can.A batch can speed of agitator is set as 800rpm, B batch can speed of agitator is 1000rpm, and C batch can speed of agitator is
1500rpm, then A, B, C batch can are respectively vacuumized and are led to nitrogen while stirring respectively, and circulation 6 times or more removals are former
Air in material, last nitrogen pressurization 0.05MPa~0.1MPa are spare.It is accurately controlled using computer-controlled closed injector
A, the respective flow of B, C batch can makes three kinds of raw materials in the mixing chamber mixed at high speed 10s of revolving speed 2000rpm, is then poured into spacious
It foams in the fixed dimension mould vehicle of mouth.After 5min when foam surface is hardened, mould vehicle is driven into large-scale microwave by guide rail and is dried
In case, power 0.35kW is set, runs 8min.Then mould vehicle continues through guide rail and drives into large-scale heated oven, setting temperature
180 DEG C of degree toasts 7h.Last mould vehicle is transported to detachment point, and removing mold can be taken off prepared polyimide foam material
Material.
Embodiment 5
According to formula isocyanates 30wt%, aromatic dianhydride 30wt%, solvent 22wt%, foaming agent 6wt%, foam stabilizer
2wt%, catalyst 1wt%, sound-absorbing material 9wt% prepare Polyimide foams.Specially take 20 parts of poly aromatic series different
Cyanate (PMDI) and 10 parts of polyphenyl polymethylene polyisocyanates (PAPI) are poured into A batch can.Take 18 parts of Pyromellitic Acids
Dianhydride and 12 part 3,3', 4,4'- diphenyl thio-ether tetrformate dianhydrides are added to 15 parts of n,N-dimethylacetamide and 7 parts of dimethyl
In the mixed solution of sulfoxide, solid is stirred at 100 DEG C and is completely dissolved.2 parts of water, 4 parts are added after system is cooled to 50 DEG C
N-Methyl pyrrolidone -600,1 part of DC6154 and 1 part of B8513, are poured into after mixing evenly in B batch can.Take 0.3 part of catalystPart catalystPart piperazine Quito pore polymer and 2 parts of PLGA polymer microballoons
With 4 parts of organic silicon rubber micro mists, poured into C batch can after mixing evenly.A batch can speed of agitator is set as 1000rpm, B batch can stirs
Mixing revolving speed is 1500rpm, and C batch can speed of agitator is 2000rpm, and then A, B, C batch can respectively carry out while stirring respectively
Vacuumize and lead to nitrogen, the air in circulation 6 times or more removal raw materials, last nitrogen pressurization 0.05MPa~0.1MPa is spare.It adopts
The respective flow of A, B, C batch can is accurately controlled with computer-controlled closed injector, makes three kinds of raw materials in revolving speed 3500rpm
Mixing chamber mixed at high speed 8s, be then poured into open fixed dimension mould vehicle and foam.When foam surface is hardened after 8min
When, mould vehicle is driven into large-scale microwave oven by guide rail, sets power 0.30kW, runs 10min.Then mould vehicle continues to lead to
It crosses guide rail to drive into large-scale heated oven, 200 DEG C of set temperature, toasts 5h.Last mould vehicle is transported to detachment point, and mold is removed
It can be taken off prepared Polyimide foams.
Comparative example 1
According to formula isocyanates 33wt%, aromatic dianhydride 33wt%, solvent 25wt%, foaming agent 6wt%, foam stabilizer
2wt%, catalyst 1wt% prepare Polyimide foams.Specially take 22 parts of poly aromatic isocyanates (PMDI) and
11 parts of polyphenyl polymethylene polyisocyanates (PAPI) are poured into A batch can.20 parts of pyromellitic acid anhydrides and 13 parts of 3,3' are taken,
4,4'- diphenyl thio-ether tetrformate dianhydrides, are added to the mixed solution of 17 parts of n,N-dimethylacetamide and 8 parts of dimethyl sulfoxides
In, solid, which is stirred to, at 100 DEG C is completely dissolved.2 parts of water, 4 parts of N-Methyl pyrrolidones-are added after system is cooled to 50 DEG C
600,1 part of DC6154 and 1 part of B8513, is poured into after mixing evenly in B batch can.Take 0.3 part of catalystWith 0.7
Part catalystIt is poured into C batch can after mixing evenly.A batch can speed of agitator is set as 1000rpm, B batch can
Speed of agitator is 1500rpm, and C batch can speed of agitator is 2000rpm, then A, B, C batch can while stirring respectively respectively into
Row vacuumizes and leads to nitrogen, the air in circulation 6 times or more removal raw materials, and last nitrogen pressurization 0.05MPa~0.1MPa is spare.
The respective flow of A, B, C batch can is accurately controlled using computer-controlled closed injector, makes three kinds of raw materials in revolving speed
The mixing chamber mixed at high speed 8s of 3500rpm is then poured into open fixed dimension mould vehicle and foams.When foam table after 8min
When face is hardened, mould vehicle is driven into large-scale microwave oven by guide rail, sets power 0.30kW, runs 10min.Then mould vehicle
It continues through guide rail to drive into large-scale heated oven, 200 DEG C of set temperature, toasts 5h.Last mould vehicle is transported to detachment point, is torn open
Except mold can be taken off prepared Polyimide foams.
Comparative example 2
According to formula isocyanates 33wt%, aromatic dianhydride 33wt%, solvent 25wt%, foaming agent 6wt%, foam stabilizer
2wt%, catalyst 1wt% prepare Polyimide foams.Specially take 22 parts of poly aromatic isocyanates (PMDI) and
11 parts of polyphenyl polymethylene polyisocyanates (PAPI) are blended together as solution one.Take 20 parts of pyromellitic acid anhydrides and
13 part 3,3', 4,4'- diphenyl thio-ether tetrformate dianhydrides are added to 17 parts of n,N-dimethylacetamide and 8 parts of dimethyl sulfoxides
In mixed solution, solid is stirred at 100 DEG C and is completely dissolved.2 parts of water, 4 parts of N- methyl are added after system is cooled to 50 DEG C
Pyrrolidones -600,1 part of DC6154,1 part of B8513,0.3 part of catalyst18 and 0.7 parts of catalystIt is used as solution two after mixing evenly.Solution one and solution two are mixed, high speed is used using convention stir
It is 3500rpm mixed at high speed 8s that revolving speed is controlled under blender air atmosphere, is then poured into open fixed dimension mould vehicle
Foaming.After 8min when foam surface is hardened, mould vehicle is driven into large-scale microwave oven by guide rail, sets power 0.30kW,
Run 10min.Then mould vehicle continues through guide rail and drives into large-scale heated oven, 200 DEG C of set temperature, toasts 5h.Finally
Mould vehicle is transported to detachment point, and removing mold can be taken off prepared Polyimide foams.
Performance test and test result
Above-described embodiment 1-5 and comparative example 1-2 polyimide foam sample prepared is measured into density respectively, is stretched by force
Degree, thermal coefficient, maximum abscess aperture and noise reduction coefficient, the data measured are as follows:
The test result that 1 embodiment 1-5 of table and comparative example 1-2 foam sample measure
As shown in Table 1, the density of Polyimide foams produced by the present invention is in 10kg/m3Left and right, tensile strength is about
60~76kPa, compressive strength about 9~12kPa have excellent mechanical property.About 0.03~0.05W/m DEG C of thermal coefficient,
With preferable thermal and insulating performance.Embodiment 1-5 compared to joined in comparative example 1-2 specifically with foam base plate compatibility
Preferable sound-absorbing material, can be uniformly dispersed in foamed material, and noise reduction coefficient 0.60 or more, can exclude making an uproar in environment
Sound has good sound absorbing performance.
(Fig. 1 is the average noise reduction coefficient of Polyimide foams prepared by the embodiment of the present invention 2 known to Fig. 1 and Fig. 3
Curve graph；Fig. 3 is the average noise reduction coefficient curve graph of Polyimide foams prepared by comparative example 1 of the present invention), system of the present invention
The Polyimide foams obtained make an uproar coefficient more than or equal to 0.60, solve existing skill by formula design and processes design etc.
The problem of the Polyimide foams sound absorption effect difference of art preparation.(Fig. 2 is that the embodiment of the present invention 2 is made known to Fig. 2 and Fig. 4
The aperture figure of standby Polyimide foams；Fig. 4 is the aperture of Polyimide foams prepared by comparative example 1 of the present invention
Figure), the maximum abscess pore diameter range of Polyimide foams produced by the present invention between 1-3 mm, the polyimides of preparation
Foamed material can have more controllable and finer and smoother foam structure.
A kind of sound absorption Polyimide foams provided by the invention and preparation method thereof, only with organic sound-absorbing material,
It can mix and be uniformly dispersed in system, production technology can not only be simplified, by changing the content of component, can also effectively adjust
Save the density of composite material, the mechanical performances such as acoustic absorptivity and Compression and Expansion, thus the application under meeting different condition.Simultaneously
It avoids and adds inorganic sound-absorbing material to the abrasion of the special gear of equipment and blocking conveyance conduit or the problems such as tube wall remains,
Be conducive to the production and maintenance of pipeline and equipment.
The present invention accurately controls each raw material proportioning using computer-controlled closed injector, and mixes in airtight cavity
It closes, compared with conventional mechanical is stirred in air, the Polyimide foams of preparation have finer and smoother foam structure.
Preparation method the degree of automation of the invention simultaneously is higher, is suitble to industrialized production.Can satisfy ships and light boats and rail traffic loss of weight,
The fields such as sound-absorption and heat-insulation, high/low temperature heat preservation, insulation fire prevention and ventilation jet chimney use the requirement of Polyimide foams.
The preferred embodiment of the present invention has shown and described in above description, as previously described, it should be understood that the present invention is not office
Be limited to form disclosed herein, should not be regarded as an exclusion of other examples, and can be used for various other combinations, modification and
Environment, and can be changed within that scope of the inventive concept describe herein by the above teachings or related fields of technology or knowledge
It is dynamic.And changes and modifications made by those skilled in the art do not depart from the spirit and scope of the present invention, then it all should be appended by the present invention
In scope of protection of the claims.
Claims (10)
1. a kind of sound absorption Polyimide foams, raw material include aromatic dianhydride, isocyanates, surfactant, foaming agent,
Catalyst, sound-absorbing material, it is characterised in that: the percentage of the raw material is isocyanate number 10%~62%, fragrance
Race's dianhydride mass fraction 15%~65%, solvent quality number 15%~35%, foaming agent mass fraction 5%~18%, even bubble
Agent mass fraction 1%~9%, catalyst quality number 0.2%~7%, sound-absorbing material mass fraction 1%~9%.
2. a kind of sound absorption Polyimide foams according to claim 1, it is characterised in that: the isocyanates is virtue
Fragrant race's isocyanates, one or more of aliphatic isocyanates and aromatic ester race isocyanates.
3. a kind of sound absorption Polyimide foams according to claim 1, it is characterised in that: the aromatic dianhydride is
Pyromellitic acid anhydride, 3,3 ' 4,4 '-benzophenone tetracarboxylic dianhydride (BTDA)s, 3,3 ' 4,4 '-diphenyl thio-ether tetrformate dianhydrides, 4 ' 4- hexichol
Ether dianhydride, 2,3,3 ', 4 '-diphenyl ether tetraformic dianhydrides, 3,3 ' 4,4 '-biphenyl dianhydrides and 3,3 ' 4,4 '-triphen bis ether tetracarboxylic acids
One or more of dianhydride；Solvent is ethyl alcohol, in dimethyl sulfoxide, N ' N-dimethylformamide, N ' N dimethyl acetamide
It is one or more of.
4. a kind of sound absorption Polyimide foams according to claim 1, it is characterised in that: the catalyst is amine
One or more of catalyst or metallic catalyst.
5. a kind of sound absorption Polyimide foams according to claim 1, it is characterised in that: organic sound-absorbing material
Including one of polymer micro mist, organosilicon microballoon, organic porous material and plant organic fiber porous material or a variety of.
6. a kind of preparation method of sound absorption Polyimide foams as described in claim 1, it is characterised in that: including following
Step,
Step 1: isocyanates is poured into A batch can；
Step 2: aromatic dianhydride is dissolved into solvent and is cooled down；
Step 3: foaming agent and foam stabilizer are added in solution made from step 2, poured into B tank after mixing evenly；
Step 4: sound-absorbing material and catalyst are poured into after mixing evenly in C tank；
Step 5: A, B, C tank are stirred respectively, by the air in vacuum nitrogen gas removal raw material；
Step 6: by the flow of computer control A, B, C batch can, by being injected into mold after the completion of closed mixing chamber mixed at high speed
Foaming, then carries out microwave treatment；
Step 7: being finally heat-treated in an oven, and mold is removed after the completion of baking can prepare the polyimides
Foamed material.
7. a kind of preparation method of Polyimide foams that absorb sound according to claim 6, it is characterised in that: the step
Solution temperature is 95-125 DEG C in rapid two, and being cooled to temperature is 25-55 DEG C.
8. a kind of preparation method of Polyimide foams that absorb sound according to claim 6, it is characterised in that: the step
A batch can speed of agitator is 10~2500rpm in rapid five, and B batch can speed of agitator is 10~2500rpm, and C batch can speed of agitator is 10
~4000rpm, mixing chamber revolving speed are 1000~4300rpm.
9. a kind of preparation method of Polyimide foams that absorb sound according to claim 6, it is characterised in that: the step
Microwave per kilogram processing power is 0.15~0.45kW in rapid six.
10. a kind of preparation method of Polyimide foams that absorb sound according to claim 6, it is characterised in that: described
Oven temperature is 160~245 DEG C in step 7.
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| CN109810251A (en) * | 2019-01-15 | 2019-05-28 | 哈尔滨工程大学 | A kind of preparation method of high-performance rigid polyimides heat insulation and acoustic absorption foam |
| CN111087618A (en) * | 2019-12-30 | 2020-05-01 | 常州天晟新材料研究院有限公司 | Sound absorption and noise reduction type polyimide foam, sound absorption and noise reduction type high-speed train cold-proof material and application |
| CN111619183A (en) * | 2020-05-20 | 2020-09-04 | 哈尔滨工程大学 | Composite polyimide foam with synergistic sound absorption effect and preparation method thereof |
| CN112126106A (en) * | 2020-09-28 | 2020-12-25 | 贵州航天天马机电科技有限公司 | High-density hard flame-retardant polyimide foam material and preparation method thereof |
| CN112745677A (en) * | 2020-12-30 | 2021-05-04 | 青岛海洋新材料科技有限公司 | High-toughness polyimide sound-absorbing foam material and preparation method thereof |
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| CN112126106A (en) * | 2020-09-28 | 2020-12-25 | 贵州航天天马机电科技有限公司 | High-density hard flame-retardant polyimide foam material and preparation method thereof |
| CN112745677A (en) * | 2020-12-30 | 2021-05-04 | 青岛海洋新材料科技有限公司 | High-toughness polyimide sound-absorbing foam material and preparation method thereof |
| CN115723285A (en) * | 2022-11-15 | 2023-03-03 | 常州福隆科技新材料有限公司 | Mold and method for preparing polyimide foam composite material by using same |
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Application publication date: 20181207 |