CN109180935A - A kind of preparation method of Polyamide-imide foam - Google Patents
A kind of preparation method of Polyamide-imide foam Download PDFInfo
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- CN109180935A CN109180935A CN201810766492.3A CN201810766492A CN109180935A CN 109180935 A CN109180935 A CN 109180935A CN 201810766492 A CN201810766492 A CN 201810766492A CN 109180935 A CN109180935 A CN 109180935A
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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
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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
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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
- C08J9/02—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by the reacting monomers or modifying agents during the preparation or modification of macromolecules
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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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- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Polyurethanes Or Polyureas (AREA)
Abstract
The invention discloses a kind of preparation methods of Polyamide-imide foam, belong to polymer synthesis method field.First diisocyanate, trimellitic anhydride, aromatic dianhydride and catalyst are added in reaction kettle by the present invention, constant temperature is stirred to react to obtain performed polymer after heating, then it pours out cooling and cooling performed polymer is crushed into obtain foam precursor using pulverizer, foam precursor is laid in mold again, high temperature foams after closed loop solidification, cooled to room temperature is stood, is demoulded to get Polyamide-imide foam material.Polyamide-imide foam material prepared by the present invention has been provided simultaneously with the resistant of high or low temperature of polyimides, from the high feature of anti-flammability, aramid strength and low cost be cheapness and solvent-free reaction and autoreaction generate CO2Foaming technique, promote its more areas promote and apply.
Description
Technical field
The invention belongs to polymer synthesis method technical fields, and it is sub- to be related to a kind of solvent-free two-step method production polyamide acyl
The method of amine foam.
Background technique
Foam of polymers is often applied to the neck such as insulation, insulation, sound insulation, damping due to the features such as density is low, light weight
Domain.Common foam of polymers be using polyolefin, polyurethane and phenolic aldehyde as the first generation of material and second generation foam of polymers, but
Intensity, temperature tolerance, physics and the chemical stability of these materials, flame resistance etc. are not able to satisfy the requirement of some special dimensions.
Typical polyimides is the polymer containing aromatic rings, aromatic heterocyclic structure, in intensity, high temperature resistant/low temperature, absolutely
Edge, chemical stabilization, it is anti-radiation, from fire-retardant, heat-insulated, noise reduction etc. have best comprehensive performance, can be used as synthetic fibers, bonding
Agent, coating agent, film, insulating film, molded item, foam, composite matrix resin and dielectric material；Especially its is outstanding
High-intensitive, high insulation, insulation, high-low temperature resistant, anti-width are penetrated, from performances such as fire-retardant and easy processings, make its space flight, aviation, navigation,
The status that material preparation in the fields such as engineering etc. has other polymers irreplaceable.
Because the outstanding properties of polyimides can remain behind in the foamed material using polyimides as material,
Polyimide foam is as having the light material that high intensity, high temperature resistant/low temperature, the third generation of fire-resistant are heat-insulated, insulate against sound,
Have and is widely applied.But due to factors such as its raw material and manufacture craft and yields, cause polyimide foam comprehensive at
This is higher, is not enough to preferably be promoted in commercial market.
Summary of the invention
Aiming at the problem that traditional foam of polymers low performance low price and polyimide foam high-performance high price, this hair
It is bright to provide a kind of preparation method of Polyamide-imide foam, for a kind of completely new, high performance-price ratio environmentally protective system
Preparation Method.
For achieving the above object, the present invention adopts the following technical scheme:
A kind of preparation method of Polyamide-imide foam, comprising the following steps:
1) 168~250 parts of diisocyanate in parts by weight, are successively taken, 125~192 parts of trimellitic anhydrides, 1~3
Part catalyst；
2) first the above-mentioned raw materials in addition to catalyst are added in reaction kettle, constant temperature is dispersed with stirring after heating, is then added
Simultaneously constant temperature mixing control reacts to obtain performed polymer catalyst, and solvent dissolution reaction is not needed in entire reaction process, is then poured out
Cooling performed polymer is simultaneously crushed to obtain foam precursor using pulverizer by cooling；
3) above-mentioned foam precursor is laid in mold, high temperature foams after imidization, stands cooled to room temperature, takes off
Mould is to get Polyamide-imide foam material.
Further, in the step 1), according to parts by weight, 0~113 part of aromatic dianhydride is weighed.
Further, the diisocyanate is with the mixture molar ratio for including trimellitic anhydride and aromatic dianhydride
100:(97-103).
Further, in the step 1), diisocyanate be '-diphenylmethane diisocyanate, toluene di-isocyanate(TDI) and
The combination of one or more of hexamethylene diisocyanate.
Further, in the step 1), aromatic dianhydride is biphenyl ether dianhydride, pyromellitic acid anhydride, biphenyl tetracarboxylic acid
Any one or the combination of several of them in acid dianhydride and benzophenone tetracarboxylic dianhydride.
Further, in the step 1), catalyst be 3- picoline, 3-ethylpyridine, pyridine, isoquinolin and 1,3,
5- tri- (DimethylAminopropyl) -1, any one or the combination of several of them in 3,5- hexahydrotriazines.Further, described to urge
Agent is 1,3,5- tri- (DimethylAminopropyl) -1,3,5- hexahydrotriazines.
Further, in the step 2), after being heated up to 135-175 DEG C, under the mixing speed of 200-800r/min into
Row constant temperature is dispersed with stirring.
Further, in the step 3), the condition of high temperature foaming is as follows: in 190-260 DEG C of baking oven, constant temperature foaming aging
60-120min。
Compared with prior art, the present invention having the advantage that
1. it is low to introduce price on the basis of giving full play to the heat resistance of high price polyimides and from anti-flammability by the present invention
Honest and clean polyamide (PA) structure, greatly reduces the overall cost of foam, and cost performance is high；
2. preparation method of the present invention uses environmentally protective synthetic technology, solvent is free of in reaction.
3. polyamide and polyimide structures perfect combination ensure that the intensity, resilience, temperature tolerance of foam by the present invention
And from features such as anti-flammabilitys, this is not available for the foam that traditional room temperature uses.
4. being not required in foaming process of the invention plus any foaming agent, foaming agent being the dioxy of generation during autoreactivity
Change the foaming of carbon gas push, is generated without other exhaust gas, waste material, while production environment is friendly.
In short, Polyamide-imide foam material prepared by the present invention has been provided simultaneously with the temperature tolerance of polyimides, has hindered certainly
The foamed stability, cheapness of combustion property and polyamide promotes it to promote and apply in more areas.
Detailed description of the invention
Fig. 1 is the FT-IR map of the Polyamide-imide foam material of preparation.
Specific embodiment
Technical solution of the present invention is described in further detail below by embodiment.The scope of the present invention is not with specific
Embodiment is limited, but is limited by the scope of the claims.
The preparation method of the Polyamide-imide foam of the present embodiment, comprising the following steps:
1) 168~250 parts of diisocyanate in parts by weight, are successively taken, 125~192 parts of trimellitic anhydrides, 0~
113 parts of aromatic dianhydrides, 1~3 part of catalyst；
2) first diisocyanate and trimellitic anhydride (and aromatic dianhydride) are added in reaction kettle, are heated up to 135-175
After DEG C, constant temperature being carried out under the mixing speed of 200-800r/min and is dispersed with stirring, catalyst is then added and continue constant temperature stirring
Performed polymer is reacted to obtain, then pour out cooling and cooling performed polymer is crushed into obtain foam precursor powder using pulverizer；
3) gained foam precursor powder is laid in mold, high temperature foams after imidization, and standing naturally cools to room
Temperature demoulds to get Polyamide-imide foam material.
Preferably, the diisocyanate in step 1) is '-diphenylmethane diisocyanate, toluene di-isocyanate(TDI) and six
The combination of one or more of methylene diisocyanate.Aromatic dianhydride is biphenyl ether dianhydride, pyromellitic acid anhydride, connection
Any one in benzene tertacarbonic acid's dianhydride and benzophenone tetracarboxylic dianhydride.Catalyst is 3- picoline, 3-ethylpyridine, pyrrole
Pyridine, isoquinolin or 1,3,5- tri- (DimethylAminopropyl) -1, one of 3,5- hexahydrotriazines or a variety of.Diisocyanate with
Mixture molar ratio including trimellitic anhydride and aromatic dianhydride is 100:(97-103).
Embodiment 1:
In parts by weight, 250 parts of '-diphenylmethane diisocyanates are successively taken, 192 parts of trimellitic anhydrides, 3 part 1,3,
5- tri- (DimethylAminopropyl) -1,3,5- hexahydrotriazines；First '-diphenylmethane diisocyanate and trimellitic anhydride are added anti-
It answers in kettle, is 135-175 DEG C in temperature, under conditions of revolving speed 200-800r/min, constant temperature stirs 3-5min, to trimellitic anhydride
After being uniformly dispersed, then reaction kettle is added in catalyst, then under conditions of 135-175 DEG C of temperature, revolving speed 200-800r/min,
After constant temperature stirs 30-60min, resin in kettle is poured out, cooled to room temperature while hot, is then consolidated cooling using pulverizer
State resin is ground into foam precursor, 60 mesh sieving for standby.Gained foam precursor is laid in mold, mold is placed in
In 190-260 DEG C of baking oven, constant temperature foaming aging 60-120min, then mold is removed into baking oven, cooled to room temperature is stood, is taken off
Mould is to get Polyamide-imide foam material.
Embodiment 2:
In parts by weight, 174 parts of toluene di-isocyanate(TDI)s are successively taken, 192 parts of trimellitic anhydrides, 2 part 1,3,5- tri-
(DimethylAminopropyl) -1,3,5- hexahydrotriazines；First toluene di-isocyanate(TDI) and trimellitic anhydride are added in reaction kettle, in
Temperature is 135-175 DEG C, and under conditions of revolving speed 200-800r/min, constant temperature stirs 3-5min, is uniformly dispersed to trimellitic anhydride
Afterwards, then by catalyst reaction kettle is added, then under conditions of 135-175 DEG C of temperature, revolving speed 200-800r/min, constant temperature stirring
After 30-60min, resin in kettle is poured out, cooled to room temperature while hot, then utilizes pulverizer by cooling solid resin powder
It is broken into foam precursor, 60 mesh sieving for standby.Gained foam precursor is laid in mold, mold is placed in 190-260 DEG C
In baking oven, constant temperature foaming aging 60-120min, then mold is removed into baking oven, cooled to room temperature is stood, demoulding is to get poly-
Amide imide foamed material.
Embodiment 3:
In parts by weight, 168 parts of hexamethylene diisocyanates are successively taken, 192 parts of trimellitic anhydrides, 1 part 1,3,
5- tri- (DimethylAminopropyl) -1,3,5- hexahydrotriazines；First hexamethylene diisocyanate and trimellitic anhydride are added anti-
It answers in kettle, is 135-175 DEG C in temperature, under conditions of revolving speed 200-800r/min, constant temperature stirs 3-5min, to trimellitic anhydride
After being uniformly dispersed, then reaction kettle is added in catalyst, then under conditions of 135-175 DEG C of temperature, revolving speed 200-800r/min,
After constant temperature stirs 30-60min, resin in kettle is poured out, cooled to room temperature while hot, is then consolidated cooling using pulverizer
State resin is ground into foam precursor, 60 mesh sieving for standby.Gained foam precursor is laid in mold, mold is placed in
In 190-260 DEG C of baking oven, constant temperature foaming aging 60-120min, then mold is removed into baking oven, cooled to room temperature is stood, is taken off
Mould is to get Polyamide-imide foam material.
Embodiment 4:
In parts by weight, 250 parts of '-diphenylmethane diisocyanates, 125 parts of trimellitic anhydrides, 76 parts of equal benzene are successively taken
Tetracarboxylic acid dianhydride, 1 part 1,3,5- tri- (DimethylAminopropyl) -1,3,5- hexahydrotriazines, 2 parts of pyridines；First by diphenyl-methane two
Isocyanates, trimellitic anhydride and pyromellitic acid anhydride are added in reaction kettle, in temperature be 135-175 DEG C, revolving speed 200-
Under conditions of 800r/min, constant temperature stirs 3-5min, after trimellitic anhydride and pyromellitic acid anhydride are uniformly dispersed, then by two
Reaction kettle is added in kind catalyst, and then under conditions of 135-175 DEG C of temperature, revolving speed 200-800r/min, constant temperature stirs 30-
After 60min, resin in kettle is poured out, cooled to room temperature while hot, is then crushed cooling solid resin using pulverizer
At foam precursor, 60 mesh sieving for standby.Gained foam precursor is laid in mold, mold is placed in 190-260 DEG C of baking
In case, constant temperature foaming aging 60-120min, then mold is removed into baking oven, cooled to room temperature is stood, is demoulded to get polyamides
Amine acid imide foam material.
Embodiment 5:
In parts by weight, 250 parts of '-diphenylmethane diisocyanates are successively taken, 125 parts of trimellitic anhydrides, 113 part two
Benzophenonetetracarboxylic dianhydride, 1 part 1,3,5- tri- (DimethylAminopropyl) -1,3,5- hexahydrotriazines, 2 parts of 3-ethylpyridines；First
By '-diphenylmethane diisocyanate, trimellitic anhydride and benzophenone tetracarboxylic dianhydride be added reaction kettle in, in temperature be 135-
175 DEG C, under conditions of revolving speed 200-800r/min, constant temperature stirs 3-5min, to trimellitic anhydride and benzophenone tetrabasic carboxylic acid two
After acid anhydride is uniformly dispersed, then reaction kettles, then in 135-175 DEG C of temperature, revolving speed 200-800r/min's are added in two kinds of catalyst
Under the conditions of, after constant temperature stirs 30-60min, resin in kettle is poured out while hot, cooled to room temperature, it then will using pulverizer
Cooling solid resin is ground into foam precursor, 60 mesh sieving for standby.Gained foam precursor is laid in mold, by mould
Tool is placed in 190-260 DEG C of baking oven, constant temperature foaming aging 60-120min, then mold is removed baking oven, and standing naturally cools to room
Temperature demoulds to get Polyamide-imide foam material.
Embodiment 6:
In parts by weight, 250 parts of '-diphenylmethane diisocyanates, 125 parts of trimellitic anhydrides, 103 parts of connection are successively taken
Benzene tertacarbonic acid's dianhydride, 1 part 1,3,5- tri- (DimethylAminopropyl) -1,3,5- hexahydrotriazines, 2 parts of 3- picolines；First by two
Phenylmethane diisocyanate, trimellitic anhydride and biphenyltetracarboxylic dianhydride are added in reaction kettle, are 135-175 DEG C in temperature, turn
Under conditions of fast 200-800r/min, constant temperature stirs 3-5min, after trimellitic anhydride and biphenyltetracarboxylic dianhydride are uniformly dispersed,
Reaction kettle is added in two kinds of catalyst again, then under conditions of 135-175 DEG C of temperature, revolving speed 200-800r/min, constant temperature is stirred
After mixing 30-60min, resin in kettle is poured out, cooled to room temperature while hot, then utilizes pulverizer by cooling solid resin
It is ground into foam precursor, 60 mesh sieving for standby.Gained foam precursor is laid in mold, mold is placed in 190-260
In DEG C baking oven, constant temperature foams aging 60-120min, then mold is removed baking oven, stands cooled to room temperature, demoulding to get
Polyamide-imide foam material.
Embodiment 7:
In parts by weight, 250 parts of '-diphenylmethane diisocyanates, 125 parts of trimellitic anhydrides, 108 parts of connection are successively taken
Phenylate dianhydride, 1 part 1,3,5- tri- (DimethylAminopropyl) -1,3,5- hexahydrotriazines, 2 parts of isoquinolin；First by diphenyl-methane two
Isocyanates, trimellitic anhydride and pyromellitic acid anhydride are added in reaction kettle, are 135-175 DEG C of revolving speed in temperature, 200-
Under conditions of 800r/min, constant temperature stirs 3-5min, after trimellitic anhydride and pyromellitic acid anhydride are uniformly dispersed, then by two
Reaction kettle is added in kind catalyst, and then under conditions of 135-175 DEG C of temperature, revolving speed 200-800r/min, constant temperature stirs 30-
After 60min, resin in kettle is poured out, cooled to room temperature while hot, is then crushed cooling solid resin using pulverizer
At foam precursor, 60 mesh sieving for standby.Gained foam precursor is laid in mold, mold is placed in 190-260 DEG C of baking
In case, constant temperature foaming aging 60-120min, then mold is removed into baking oven, cooled to room temperature is stood, is demoulded to get polyamides
Amine acid imide foam material.
Embodiment 8:
In parts by weight, 125 parts of '-diphenylmethane diisocyanates are successively taken, 87 parts of toluene di-isocyanate(TDI)s, 192 parts
Trimellitic anhydride, 2 part 1,3,5- tri- (DimethylAminopropyl) -1,3,5- hexahydrotriazines；First by '-diphenylmethane diisocyanate,
Toluene di-isocyanate(TDI) and trimellitic anhydride are added in reaction kettle, in temperature be 135-175 DEG C, the item of revolving speed 200-800r/min
Under part, constant temperature stirs 3-5min, reaction kettle is added after trimellitic anhydride is uniformly dispersed, then by catalyst, then in temperature
135-175 DEG C, under conditions of revolving speed 200-800r/min, after constant temperature stirs 30-60min, resin in kettle is poured out while hot, it is natural
It is cooled to room temperature, cooling solid resin is then ground into foam precursor, 60 mesh sieving for standby using pulverizer.By gained
Foam precursor is laid in mold, and mold is placed in 190-260 DEG C of baking oven, and constant temperature foams aging 60-120min, then by mould
Tool removes baking oven, stands cooled to room temperature, demoulds to get Polyamide-imide foam material.
Embodiment 9:
In parts by weight, 125 parts of '-diphenylmethane diisocyanates are successively taken, 84 parts of hexamethylene diisocyanates,
192 parts of trimellitic anhydrides, 2 part 1,3,5- tri- (DimethylAminopropyl) -1,3,5- hexahydrotriazines；First by two isocyanide of diphenyl-methane
Acid esters, hexamethylene diisocyanate and trimellitic anhydride are added in reaction kettle, in temperature be 135-175 DEG C, revolving speed 200-
Under conditions of 800r/min, constant temperature stirs 3-5min, and reaction kettle is added after trimellitic anhydride is uniformly dispersed, then by catalyst,
Then under conditions of 135-175 DEG C of temperature, revolving speed 200-800r/min, after constant temperature stirs 30-60min, resin in kettle is taken advantage of
Heat is poured out, cooled to room temperature, and cooling solid resin is then ground into foam precursor, the sieving of 60 mesh using pulverizer
It is spare.Gained foam precursor is laid in mold, mold is placed in 190-260 DEG C of baking oven, constant temperature foaming aging 60-
120min, then mold is removed into baking oven, cooled to room temperature is stood, is demoulded to get Polyamide-imide foam material.
Embodiment 10:
In parts by weight, 87 parts of toluene di-isocyanate(TDI)s are successively taken, 84 parts of hexamethylene diisocyanates, 192 parts
Trimellitic anhydride, 1 part 1,3,5- tri- (DimethylAminopropyl) -1,3,5- hexahydrotriazines；First by toluene di-isocyanate(TDI), six Asias
Methyl diisocyanate and trimellitic anhydride are added in reaction kettle, in temperature be 135-175 DEG C, the item of revolving speed 200-800r/min
Under part, constant temperature stirs 3-5min, reaction kettle is added after trimellitic anhydride is uniformly dispersed, then by catalyst, then in temperature
135-175 DEG C, under conditions of revolving speed 200-800r/min, after constant temperature stirs 30-60min, resin in kettle is poured out while hot, it is natural
It is cooled to room temperature, cooling solid resin is then ground into foam precursor, 60 mesh sieving for standby using pulverizer.By gained
Foam precursor is laid in mold, and mold is placed in 190-260 DEG C of baking oven, and constant temperature foams aging 60-120min, then by mould
Tool removes baking oven, stands cooled to room temperature, demoulds to get Polyamide-imide foam material.
Above-mentioned 10 kinds of embodiments can react system bubble, but slightly different for the density of abscess, intensity.
As shown in Figure 1, the FT-IR map of the Polyamide-imide foam material for preparation:
In FT-IR spectrogram, in 3325.65cm-1It is the stretching vibration peak of amide N-H that, which there is a broad peak at place,；
1776.80cm-1, 1712.94cm-1The symmetrical and asymmetric stretching vibration absworption peak of respectively imine structure-CO-N-CO-；
1662.48cm-1For the stretching vibration absworption peak of C=O in amide；1597.86cm-1, 1510.17cm-1For the skeletal vibration of phenyl ring
Absorption peak；1370.32cm-1For the stretching vibration absworption peak of C-N in imines；721.55cm-1For in imines-CO-N-CO- it is curved
Bent vibration absorption peak, information above prove that the polymer of preparation is polyamidoimide.
Following table is the Polyamide-imide foam material characterization data of preparation.
Table 1 (representative value)
| Density Kg/m3 | Tensile strength kPa | Oxygen index (OI) % | Thermal coefficient W/ (m*K) |
| 8~40 | ≥210 | ≥31.3 | 0.040 |
It should be understood that above-described embodiment is only the preferred embodiment of the present invention, for illustrating the specific of technical solution of the present invention
Embodiment, rather than limit the scope of the invention.It is noted that, after the present invention has been read, those skilled in the art
Without departing from the principle of the present invention, several improvement and equivalent replacement can also be made, these are to of the invention various etc.
Modification and replacement with form fall within protection scope defined by the claim of this application.
Claims (9)
1. a kind of preparation method of Polyamide-imide foam, which is characterized in that the described method comprises the following steps:
1) 168~250 parts of diisocyanate in parts by weight, are successively taken, 125~192 parts of trimellitic anhydrides, 1~3 part is urged
Agent；
2) first the above-mentioned raw materials in addition to catalyst are added in reaction kettle, constant temperature is dispersed with stirring after heating, and catalysis is then added
Simultaneously constant temperature mixing control reacts to obtain performed polymer for agent, then pours out cooling and crushes cooling performed polymer to obtain bubble using pulverizer
Foam presoma；
3) above-mentioned foam precursor being laid in mold, high temperature foams after imidization, stands cooled to room temperature, it demoulds,
Up to Polyamide-imide foam material.
2. a kind of preparation method of Polyamide-imide foam according to claim 1, which is characterized in that the step 1)
In, according to parts by weight, weigh 0~113 part of aromatic dianhydride.
3. a kind of preparation method of Polyamide-imide foam according to claim 2, which is characterized in that two isocyanide
The molar ratio of acid esters and the mixture for including trimellitic anhydride and aromatic dianhydride is 100:(97-103).
4. according to claim 1-3 it is one of any described in a kind of Polyamide-imide foam preparation method, which is characterized in that
In the step 1), diisocyanate is '-diphenylmethane diisocyanate, toluene di-isocyanate(TDI) and hexa-methylene diisocyanate
The combination of one or more of ester.
5. according to claim 1-3 it is one of any described in a kind of Polyamide-imide foam preparation method, which is characterized in that
In the step 1), aromatic dianhydride is biphenyl ether dianhydride ODPA, pyromellitic acid anhydride PMDA, biphenyltetracarboxylic dianhydride BPDA
With any one in benzophenone tetracarboxylic dianhydride BTDA.
6. according to claim 1-3 it is one of any described in a kind of Polyamide-imide foam preparation method, which is characterized in that
In the step 1), catalyst is 3- picoline, 3-ethylpyridine, pyridine, isoquinolin and 1,3,5- tri- (dimethyl amines third
Base) -1, any one or the combination of several of them in 3,5- hexahydrotriazines.
7. a kind of preparation method of Polyamide-imide foam according to claim 6, which is characterized in that the catalyst
It is 1,3,5- tri- (DimethylAminopropyl) -1,3,5- hexahydrotriazines.
8. according to claim 1-3 it is one of any described in a kind of Polyamide-imide foam preparation method, which is characterized in that
In the step 2), after being heated up to 135-175 DEG C, constant temperature is carried out under the mixing speed of 200-800r/min and is dispersed with stirring.
9. according to claim 1-3 it is one of any described in a kind of Polyamide-imide foam preparation method, which is characterized in that
In the step 3), the condition of high temperature foaming is as follows: in 190-260 DEG C of baking oven, constant temperature foaming aging 60-120min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201810766492.3A CN109180935A (en) | 2018-07-12 | 2018-07-12 | A kind of preparation method of Polyamide-imide foam |
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| CN201810766492.3A CN109180935A (en) | 2018-07-12 | 2018-07-12 | A kind of preparation method of Polyamide-imide foam |
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| CN (1) | CN109180935A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| 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 |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4980387A (en) * | 1989-07-13 | 1990-12-25 | Manville Corporation | Lightweight flexible imide foam and method of producing same |
| CN103214688A (en) * | 2013-05-10 | 2013-07-24 | 中国科学院长春应用化学研究所 | Polyamide-imide foam and preparation method thereof |
-
2018
- 2018-07-12 CN CN201810766492.3A patent/CN109180935A/en not_active Withdrawn
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4980387A (en) * | 1989-07-13 | 1990-12-25 | Manville Corporation | Lightweight flexible imide foam and method of producing same |
| CN103214688A (en) * | 2013-05-10 | 2013-07-24 | 中国科学院长春应用化学研究所 | Polyamide-imide foam and preparation method thereof |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN109810251B (en) * | 2019-01-15 | 2021-10-26 | 哈尔滨工程大学 | Preparation method of high-performance rigid polyimide heat-insulation sound-absorption foam |
| 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 |
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