CN109810251A - A kind of preparation method of high-performance rigid polyimides heat insulation and acoustic absorption foam - Google Patents
A kind of preparation method of high-performance rigid polyimides heat insulation and acoustic absorption foam Download PDFInfo
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Abstract
A kind of preparation method of high-performance rigid polyimides heat insulation and acoustic absorption foam, belongs to technical field of polymer materials.The present invention includes: that polyisocyanates is dissolved in polar solvent under the conditions of nitrogen protection, and aromatic anhydride is then added, and reaction obtains the thick polyimide precursor solution containing seven-members ring structure;Surfactant is added into sticky system, the reaction was continued obtains sticky paste foaming presoma;The foaming presoma with certain self-supporting hardness will be formed after the resting for a few days polymerization thickening of sticky paste foaming presoma;Foaming presoma microwave treatment is obtained into the harder foam intermediate of quality;High-performance rigid polyimides heat insulation and acoustic absorption foamed material is obtained through hot setting finally, foam intermediate is placed in high temperature oven.High-performance rigid polyimides heat insulation and acoustic absorption foam performance prepared by the present invention is excellent, and the cost of raw material needed for preparing is cheap and selectable range is wider, and preparation process is simple and easy to do, is conducive to industrialized production and extensive use.
Description
Technical field
The invention belongs to technical field of polymer materials, and in particular to a kind of high-performance rigid polyimides heat insulation and acoustic absorption bubble
The preparation method of foam.
Background technique
Polyimide foams due to excellent lower temperature resistance, heat resistance, dielectricity, anti-flammability, using safe
The performances such as property, corrosion resistance and heat insulation and acoustic absorption, are important a member in high performance polymer material.In order to meet aviation boat
It, the demand of the fields to novel high-performance porous heat-insulating sound absorption structure functional material such as naval vessel, high-performance rigid polyimides every
Extensive concern of the development of hot acoustic foam by numerous scientific research personnel.
It is less about the development report of high-performance backbone chain type hard polyimide heat insulation and acoustic absorption foamed material at present, it is most of
In terms of research work all concentrates on side-chain polyimide foam-polymethacrylimide foam (PMI), and PMI foam by
The limitation of main chain lard type molecular structure, heat resistance, anti-flammability and in terms of performance it is poor, aviation is not achieved
The sophisticated technologies field such as space flight, naval vessel is to the technical requirements of high temperature resistant, functional material safe to use, while sound absorbing performance
Also poor.The patents such as CN103524968A, CN1610719A disclose the method for improving PMI foam safety in utilization in succession, but
Backbone chain type polyimide foam high temperature resistant and fire-retardant level is still not achieved.
In high-intensitive backbone chain type polyimide foam field, the patents such as US5077318, US6180746 report in succession according to
Hold in the palm the methods of the microwave of polyimide foam powder method technology of preparing, microballoon, molding, while CN102127225A,
The patents such as CN102127225A, CN105315464B also report the die pressing for relying on polyimide foam Water blown technology of preparing
And the method for being first molded again microwave sizing.It although can effectively ensure that material thermal resistance based on powder method technology of preparing and using peace
Quan Xing, but the cost of raw material is higher, the production cycle is longer, preparation process is complicated and obtained material mechanical performance is general
It is lower, substantially in 3MPa or less.Using multi-anhydride and isocyanates as raw material, the mould pressing technology based on Water blown technology can
Effectively promote material mechanical performance, 350kg/m3Above material compressive strength generally all in 10MPa, has preparation process letter
Singly, the advantages that cost of raw material is cheap, with short production cycle, therefore it is more conducive to the realization of industrialized production, but to equipment
It is more demanding, and operating process is more dangerous, while Water blown technical process is easy to produce the by-products such as a large amount of urea groups, leads
It causes the safety in utilization of material to be declined compared to powder law technology, limits it and further develop.The patents such as US3300420 are public
Cloth is using multi-anhydride and isocyanates as raw material, based on the technology path of non-aqueous foaming technique technology of preparing imines foam,
Obtained material thermal resistance and safety in utilization are higher, but since expansion ratio is higher, while foamed forming process is relatively simple,
Obtained material mechanical performance is poor and frangible, is unfavorable for practical application, can not make as high-strength structure functional material
With.
Summary of the invention
The purpose of the present invention is to provide a kind of high-performance for preparing safety in utilization, heat resistance and good heat stability is hard
The preparation method of matter polyimides heat insulation and acoustic absorption foam.It is sub- by polyamides under microwave and hot conditions using non-water blown system
Amine heptatomic ring shape presoma is converted to carbon dioxide released in imide ring process and the solvent of remnants realizes foaming
And imidization, finally obtain high-performance rigid polyimides heat insulation and acoustic absorption foam.In synthesis, standing, foaming and Asia
Anhydrous participation, avoids the generation of urea groups in the several links of amination, has reached the safety of guarantee materials'use, heat resistance and heat
The purpose of stability.Meanwhile presoma itself viscosity that foams is larger, effectively reduces expansion ratio, shows final material
Higher density is laid a good foundation for the high intensity of material.Preparation for high-performance rigid polyimides heat insulation and acoustic absorption foam mentions
New thinking has been supplied, while having established technical foundation for the preparation of high-performance heat insulation and acoustic absorption integrated function structural material.
The object of the present invention is achieved like this:
The mass fraction group of a kind of preparation method of high-performance rigid polyimides heat insulation and acoustic absorption foam, material becomes polyisocyanate
60-100 parts of cyanate, 150-300 parts of polar solvent, 50-120 parts of aromatic dianhydride, 1-15 parts of surfactant, it is specific to make
It is standby the following steps are included:
(1) polar solvent pre-processed through vacuum distillation purification is added into flask, is then placed into flask pre-
It is first heated in 30-70 DEG C of oil bath pan, accesses nitrogen protection device, be then gradually added into isocyanates, under mechanical stirring
It is sufficiently mixed, obtains homogeneous phase solution;
(2) 100-300rpm is set by churned mechanically revolving speed, is added while stirring into homogeneous phase solution dry through vacuum
The aromatic dianhydride of 8-12h was pre-processed under the conditions of 90-120 DEG C of dry case into reaction system, was stirred to react 2-8 hours, until anti-
It should be become viscous to system solution;
(3) surfactant is added into sticky reaction system, continues to stop instead to after there is obvious lines for stirring 2-6 hours
It answers, paste sticky in flask foaming presoma is taken out and sealing and standing saves, it is stand-by after its polymerization thickening 5-10 days;
(4) the foaming presoma saved will be stood to be put into the microwave equipment of 500-3000W, after microwave treatment 5-40min,
Obtain the harder foam intermediate of quality;
(5) foam intermediate is taken out from microwave equipment, and be immediately placed in be previously heated to 200-300 DEG C high temperature it is dry
20-90min is post-processed in dry case, high-performance rigid polyimides heat insulation and acoustic absorption foamed material is prepared.
The polar solvent are as follows: N-Methyl pyrrolidone (NMP), n,N-Dimethylformamide (DMF), N, N- dimethyl
The highly polar aprotic solvent such as acetamide (DMAc).
The monomer of the polyisocyanates is any one or a few in compound listed by following (1)~(14):
Wherein ,-NCO is-N=C=O.
The monomer of the aromatic dianhydride is any one or a few in compound listed by following (1)~(15):
The surfactant are as follows: the non-hydrolytic type water soluble polyether siloxanes of AK or DC series, Zonyl series non-ionic
Fluorocarbon surfactant, PEG series polyoxyethylene nonionic surfactant etc..
The beneficial effects of the present invention are:
With the existing technology road for realizing material mechanical performance promotion by using closed container restraint of liberty expansion ratio
Line is compared, excellent performance of polyimide material itself has not only been effectively ensured in the present invention, but also enormously simplifies promotion material
The technique of mechanical property provides new thinking for the preparation of high-performance rigid polyimide foam.High property of the present invention
Energy hard polyimide heat insulation and acoustic absorption foam performance is excellent, and compressive strength is reached up to 5MPa or more, glass transition temperature
To 330 DEG C or more, acoustic absorptivity is more than 0.6;The cost of raw material needed for preparing is cheap and selectable range is wider, preparation process letter
Easy row, is conducive to industrialized production and extensive use;It can be used as the neck such as communications and transportation, aerospace, naval vessel, weapon, engineering
The structural foam in domain is widely used.
Detailed description of the invention
Fig. 1 is that polyimide foam compression stress strain curve is made in embodiment 1 under different condition;
Fig. 2 is that polyimide foam compression stress is made in embodiment 4-8 under the conditions of different surfaces activating agent additive amount
Strain curve;
Fig. 3 is that polyimide foam scanning electron microscope is made in embodiment 4-8 under the conditions of different surfaces activating agent additive amount
Photo;
Fig. 4 is the compressive strength histogram of embodiment 4-8.
Specific embodiment
The present invention is described in more detail with reference to the accompanying drawing.
A kind of preparation method of high-performance rigid polyimides heat insulation and acoustic absorption foam, comprising the following steps:
(1) polar solvent pre-processed through vacuum distillation purification is added into flask, is then placed into flask pre-
It is first heated in 30-70 DEG C of oil bath pan, accesses nitrogen protection device, be then gradually added into isocyanates, under mechanical stirring
It is sufficiently mixed, obtains homogeneous phase solution.
(2) 100-300rpm is set by churned mechanically revolving speed, is added while stirring into homogeneous phase solution dry through vacuum
The aromatic dianhydride of 8-12h was pre-processed under the conditions of 90-120 DEG C of dry case into reaction system, was stirred to react 2-8 hours, until anti-
It should be become viscous to system solution.
(3) surfactant is added into sticky reaction system, continues to stop instead to after there is obvious lines for stirring 2-6 hours
It answers, paste sticky in flask foaming presoma is taken out and sealing and standing is saved into after one-step polymerization thickens 5-10 days for use.
(4) the foaming presoma saved will be stood to be put into the microwave equipment of 500-3000W, after microwave treatment 5-40min,
Obtain the harder foam intermediate of quality.
(5) foam intermediate is taken out from microwave equipment, and be immediately placed in be previously heated to 200-300 DEG C high temperature it is dry
20-90min is post-processed in dry case, high-performance rigid polyimides heat insulation and acoustic absorption foamed material is prepared.
The present invention may also include:
1, the mass fraction group of the material becomes polyisocyanates 60-100 parts, 150-300 parts of polar solvent, fragrance two
50-120 parts of acid anhydride, 1-15 parts of surfactant.
2, the polar solvent includes: N-Methyl pyrrolidone (NMP), n,N-Dimethylformamide (DMF), N, N- bis-
The highly polar aprotic solvent such as methylacetamide (DMAc).
3, the multicomponent isocyanate monomer includes '-diphenylmethane diisocyanate, toluene di-isocyanate(TDI), to benzene two
Any one or a few in the polyisocyanates such as isocyanates, poly methylene poly phenyl poly isocyanate.
4, the aromatic dianhydride monomer be pyromellitic acid anhydride, benzophenone tetracarboxylic dianhydride, diphenyl ether tetracid dianhydride,
Any one or a few in the dianhydride monomers such as biphenyltetracarboxylic dianhydride.
5, the surfactant are as follows: the non-hydrolytic type water soluble polyether siloxanes of AK or DC series, Zonyl series it is non-from
Sub- fluorocarbon surfactant, PEG series polyoxyethylene nonionic surfactant etc..
In the technical system for preparing polyimide foam as raw material using multi-anhydride and isocyanates often using water as
Foaming agent, polyether polyols alcohols realizes foamed forming process as surfactant, but can draw in matrix resin molecular structure
Entering the by-products such as a large amount of urea groups, urethano leads to the decline of material thermal resistance and safety in utilization, is unable to reach tradition with two
Acid anhydride and diamines use polyimide foam performance state made from powder method.If by multi-anhydride and polyisocyanates in advance in pole
Property solvent in reaction formed have seven-members ring structure polyimides intermediate and foaming presoma, by microwave and high-temperature process
The carbon dioxide realization that the solvent volatilization and seven-members ring structure imidization of residual solvent are released in system in the process is foamed into
Type process can then substantially reduce the production quantity of the by-products such as urea groups, guarantee the safety in utilization and heat resistance of material entirety.Simultaneously
Guaranteeing on materials'use safety and heat resistance basis, to realize high-performance heat insulation and acoustic absorption integrated function structural material
Preparation, present invention firstly provides first further polymerize multi-anhydride and polyisocyanates pre-polymerization after thickening using standing
It is formed with the mode of the foaming presoma of certain self-supporting hardness, realizes binding force in foaming presoma viscosity and foaming process
Significantly promotion, solve that traditional approach foaming process medium viscosity is too low to make that its expansion ratio is excessively high, abscess hole wall is excessively thin, from
And it is made not have the problem of load bearing ability, the mechanical property of density of material and final material has been effectively ensured.Through micro-
Involve heat resistance and mechanical property that hot setting double process further ensures material.
With the existing technology road for realizing material mechanical performance promotion by using closed container restraint of liberty expansion ratio
Line is compared, excellent performance of polyimide material itself has not only been effectively ensured in the present invention, but also enormously simplifies promotion material
The technique of mechanical property provides new thinking for the preparation of high-performance rigid polyimide foam.High property of the present invention
Energy hard polyimide heat insulation and acoustic absorption foam performance is excellent, and compressive strength is reached up to 5MPa or more, glass transition temperature
To 330 DEG C or more, acoustic absorptivity is more than 0.6;The cost of raw material needed for preparing is cheap and selectable range is wider, preparation process letter
Easy row, is conducive to industrialized production and extensive use, has achieved the purpose that invention.It can be used as communications and transportation, aerospace, warship
The structural foam in the fields such as ship, weapon, engineering is widely used.
The present invention is described in further detail by the following examples, not limits range according to the present invention.
Embodiment 1
3,3',4,4' benzophenone tetracarboxylic dianhydride (BTDA) monomer powders are placed in a vacuum drying oven 100 DEG C of processing
12 hours;Aprotic polar solvent N,N-dimethylformamide (DMF) is evaporated under reduced pressure and is purified;Polymethylene polyphenyl polyisocyanate cyanogen
It is not processed before acid esters (PAPI) use.The DMF of 60.0g is added in 250mL flask with three necks,round bottom, preparatory heating is placed into
Into 40 DEG C of oil bath pans, nitrogen protection device is loaded, and instill 27.0g PAPI dropwise after being passed through nitrogen 1min, in machinery
It is sufficiently mixed under stirring, obtains beige homogeneous phase solution.
200rpm is set by churned mechanically revolving speed, the BTDA monomer of 33.0g is added while stirring into reaction system,
System solution becomes viscous after reaction 5 hours.Then, be added 3.0g surfactant A K-8805, continue stirring 4 hours it is bright to having
Stop reaction after aobvious lines.Sticky paste foaming presoma in there-necked flask is taken out and sealed, 10 are kept in dark place at room temperature
It.
The foaming presoma for having certain self-supporting strength is put into microwave equipment, sets 700W for microwave power, is located
The foam intermediate material of the harder polyimide foam of quality is obtained after reason 5min.Foam intermediate is taken from microwave equipment
Out, it and is immediately placed in the high-temperature blast drying oven for be previously heated to 260 DEG C and post-processes 30min, obtain high-performance rigid polyamides
Imines foam heat-insulating acoustic foams.
Obtained high-performance rigid polyimide foam heat insulation and acoustic absorption foam performance is as follows:
Density: 212kg/m3;Compressive strength: 1.2MPa;Compression modulus: 11.2MPa;Glass transition temperature: 333 DEG C;
10% decomposition temperature: 543 DEG C;Thermal coefficient: 0.056W/mK;Average sound absorption coefficient: 0.65.
In contrast, the foaming presoma for having certain self-supporting strength is simply placed in microwave equipment, microwave power 700W,
5min is handled, and does not carry out high-temperature blast drying and post-processes the harder polyimide foam of obtained quality, performance is as follows:
Density: 220kg/m3;Compressive strength: 1.0MPa;Compression modulus: 5.4MPa;10% decomposition temperature: 452 DEG C.The decomposition temperature of material
Degree and mechanical property, which have, largely to be declined.
In contrast, by the foaming presoma for having certain self-supporting strength only in 260 DEG C of high-temperature blast drying oven after
The polyimide foam that processing 30min is obtained, performance are as follows: density: 157kg/m3;Compressive strength: 0.4MPa;Compress mould
Amount: 5.7MPa;10% decomposition temperature: 520 DEG C.The decomposition temperature of material is slightly decreased, but mechanical properties decrease 60%.
Illustrate, pre-processed through microwave, then obtained polyimide foam can be shown well after high-temperature process
Heat resistance, thermal stability and mechanical property.
Embodiment 2
Embodiment 1 is changed to: the DMF of 40.0g is added in 250mL flask with three necks,round bottom.
Obtained high-performance rigid polyimide foam heat insulation and acoustic absorption foam performance is as follows:
Density: 235kg/m3;Compressive strength: 1.9MPa;Compression modulus: 29MPa;10% decomposition temperature: 550 DEG C;It is thermally conductive
Coefficient: 0.053W/mK;Average sound absorption coefficient: 0.62.
Embodiment 3
3,3',4,4' benzophenone tetracarboxylic dianhydride (BTDA) monomer powders are placed in a vacuum drying oven 100 DEG C of processing
12 hours;Aprotic polar solvent N,N-dimethylformamide (DMF) is evaporated under reduced pressure and is purified;Polymethylene polyphenyl polyisocyanate cyanogen
It is not processed before acid esters (PAPI) use.The DMF of 40.0g is added in 250mL flask with three necks,round bottom, preparatory heating is placed into
Into 50 DEG C of oil bath pans, nitrogen protection device is loaded, and instill 27.0g PAPI dropwise after being passed through nitrogen 1min, in machinery
It is sufficiently mixed under stirring, obtains beige homogeneous phase solution.
200rpm is set by churned mechanically revolving speed, the BTDA monomer of 33.0g is added while stirring into reaction system,
System solution becomes viscous after reaction 4 hours.Then, be added 3.0g surfactant A K-8805, continue stirring 5 hours it is bright to having
Stop reaction after aobvious lines.Sticky paste foaming presoma in there-necked flask is taken out and sealed and is kept in dark place at room temperature 8 days.
The foaming presoma for having certain self-supporting strength is put into microwave equipment, sets 700W for microwave power, is located
The foam intermediate material of the harder polyimide foam of quality is obtained after reason 5min.Foam intermediate is taken from microwave equipment
Out, it and is immediately placed in the high-temperature blast drying oven for be previously heated to 260 DEG C and post-processes 30min, obtain high-performance rigid polyamides
Imines foam heat-insulating acoustic foams.
Obtained high-performance rigid polyimide foam heat insulation and acoustic absorption foam performance is as follows:
Density: 256kg/m3;Compressive strength: 2.6MPa;Compression modulus: 30.7MPa;Glass transition temperature: 342 DEG C;
10% decomposition temperature: 544 DEG C;Thermal coefficient: 0.063W/mK;Average sound absorption coefficient: 0.60.
Embodiment 4
3,3',4,4' benzophenone tetracarboxylic dianhydride (BTDA) monomer powders are placed in a vacuum drying oven 100 DEG C of processing
12 hours;Aprotic polar solvent N,N-dimethylformamide (DMF) is evaporated under reduced pressure and is purified;Polymethylene polyphenyl polyisocyanate cyanogen
It is not processed before acid esters (PAPI) use.The DMF of 40.0g is added in 250mL flask with three necks,round bottom, preparatory heating is placed into
Into 50 DEG C of oil bath pans, nitrogen protection device is loaded, and instill 27.0g PAPI dropwise after being passed through nitrogen 1min, in machinery
It is sufficiently mixed under stirring, obtains beige homogeneous phase solution.
200rpm is set by churned mechanically revolving speed, the BTDA monomer of 33.0g is added while stirring into reaction system,
System solution becomes viscous after reaction 3 hours.Then, be added 1.2g surfactant A K-8805, continue stirring 5 hours it is bright to having
Stop reaction after aobvious lines.Sticky paste foaming presoma in there-necked flask is taken out and sealed, 10 are kept in dark place at room temperature
It.
The foaming presoma for having certain self-supporting strength is put into microwave equipment, sets 700W for microwave power, is located
The foam intermediate material of the harder polyimide foam of quality is obtained after reason 5min.Foam intermediate is taken from microwave equipment
Out, it and is immediately placed in the high-temperature blast drying oven for be previously heated to 260 DEG C and post-processes 30min, obtain high-performance rigid polyamides
Imines foam heat-insulating acoustic foams.
Embodiment 5
Embodiment 4 is changed to: then, 2.4g surfactant A K-8805 is added, continue stirring 5 hours it is obvious to having
Stop reaction after lines.
Embodiment 6
Embodiment 4 is changed to: then, 3.6g surfactant A K-8805 is added, continue stirring 5 hours it is obvious to having
Stop reaction after lines.
Embodiment 7
Embodiment 4 is changed to: then, 4.8g surfactant A K-8805 is added, continue stirring 5 hours it is obvious to having
Stop reaction after lines.
Embodiment 8
Embodiment 4 is changed to: then, 6.0g surfactant A K-8805 is added, continue stirring 5 hours it is obvious to having
Stop reaction after lines.
Obtained high-performance rigid polyimide foam heat insulation and acoustic absorption foam performance such as following table institute in embodiment 4-8
Show.
Claims (5)
1. a kind of preparation method of high-performance rigid polyimides heat insulation and acoustic absorption foam, it is characterised in that: the mass fraction of material
Group becomes polyisocyanates 60-100 parts, 150-300 parts of polar solvent, 50-120 parts of aromatic dianhydride, 1-15 parts of surfactant,
Its specific preparation the following steps are included:
(1) polar solvent pre-processed through vacuum distillation purification is added into flask, then flask is placed into and is added in advance
Heat accesses nitrogen protection device, is then gradually added into isocyanates, under mechanical stirring sufficiently into 30-70 DEG C of oil bath pan
Mixing, obtains homogeneous phase solution;
(2) 100-300rpm is set by churned mechanically revolving speed, vacuum dried case is added into homogeneous phase solution while stirring
The aromatic dianhydride of 8-12h was pre-processed under the conditions of 90-120 DEG C into reaction system, was stirred to react 2-8 hours, until reaction is extremely
System solution becomes viscous;
(3) surfactant is added into sticky reaction system, continues to stop reaction to after there is obvious lines in stirring 2-6 hours,
Paste sticky in flask foaming presoma is taken out and sealing and standing saves, it is stand-by after its polymerization thickening 5-10 days;
(4) the foaming presoma saved will be stood to be put into the microwave equipment of 500-3000W, after microwave treatment 5-40min, is obtained
The harder foam intermediate of quality;
(5) foam intermediate is taken out from microwave equipment, and is immediately placed in and is previously heated to 200-300 DEG C of high temperature drying case
High-performance rigid polyimides heat insulation and acoustic absorption foamed material is prepared in middle post-processing 20-90min.
2. a kind of preparation method of high-performance rigid polyimides heat insulation and acoustic absorption foam according to claim 1, feature
It is: the polar solvent are as follows: N-Methyl pyrrolidone (NMP), n,N-Dimethylformamide (DMF), N, N- dimethyl second
The highly polar aprotic solvent such as amide (DMAc).
3. a kind of preparation method of high-performance rigid polyimides heat insulation and acoustic absorption foam according to claim 1, feature
Be: the monomer of the polyisocyanates is any one or a few in compound listed by following (1)~(14):
Wherein ,-NCO is-N=C=O.
4. a kind of preparation method of high-performance rigid polyimides heat insulation and acoustic absorption foam according to claim 1, feature
Be: the monomer of the aromatic dianhydride is any one or a few in compound listed by following (1)~(15):
5. a kind of preparation method of high-performance rigid polyimides heat insulation and acoustic absorption foam according to claim 1, feature
It is: the surfactant are as follows: the non-hydrolytic type water soluble polyether siloxanes of AK or DC series, Zonyl series non-ionic fluorine
Carbon surface active agent, PEG series polyoxyethylene nonionic surfactant etc..
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