CN111548491A - Solvent-free preparation method of polyimide foam and product - Google Patents
Solvent-free preparation method of polyimide foam and product Download PDFInfo
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- CN111548491A CN111548491A CN202010441329.7A CN202010441329A CN111548491A CN 111548491 A CN111548491 A CN 111548491A CN 202010441329 A CN202010441329 A CN 202010441329A CN 111548491 A CN111548491 A CN 111548491A
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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
- C08J9/12—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
- C08J9/125—Water, e.g. hydrated salts
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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
- C08J2203/10—Water or water-releasing compounds
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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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Abstract
The invention discloses a solvent-free preparation method of polyimide foam and a product, wherein the preparation method comprises the following steps of 1) uniformly mixing a foaming agent, a surfactant and a catalyst to prepare a compound material; 2) uniformly mixing polyisocyanate and polybasic aromatic anhydride, and reacting for a period of time to obtain polyimide intermediate slurry; 3) uniformly mixing the compound material and the polyimide intermediate slurry to obtain foaming slurry; 4) pouring the foaming slurry into a foaming mold, immediately placing the foaming mold in a vacuum oven, and slowly foaming and molding under the conditions of negative pressure and high temperature to obtain a foam intermediate; 5) and (3) shaping the foam intermediate in a vacuum oven, and curing at high temperature to obtain the soft solvent-free polyimide foam. The invention does not use polar solvent in the whole preparation process, not only reduces the production cost, but also fundamentally avoids the harm of the polar solvent to the environment and the human health, is beneficial to industrial production and wide application, and achieves the aim of the invention.
Description
Technical Field
The invention relates to the technical field of polymer foam preparation, in particular to a solvent-free preparation method of polyimide foam and a product.
Background
The polyimide foam has the characteristics of low density, light weight, fire resistance, heat insulation and sound absorption, and is widely applied to multiple fields of high-end automobiles, high-speed trains, aerospace, navigation ships and warships and the like. According to different preparation methods, the current polyimide foams are mainly divided into a one-step polyimide foam preparation route and a two-step polyimide foam preparation route. Both of these preparations do not avoid the use of a large amount of polar solvents due to the low solubility of the anhydride derivative and the polyesterammonium polyimideaf. Furan, amide and alkanone polar solvent have effects such as violent volatilization and schizolysis in the foam high temperature preparation process, if retrieve and handle not scientifically incomplete, not only can cause serious harm to production personnel's health, still can cause serious pollution to the environment to the polar solvent who remains in the foam also can volatilize gradually in the use, and long-term the use will influence user's health, will influence the wide application of polyimide foam in the most advanced technical field finally. Meanwhile, the use of a large amount of polar solvent directly increases the preparation cost and post-treatment cost of the material, which is not favorable for further cost reduction of the polyimide foam material.
The emission of polar solvents and pyrolysis products thereof including carbon monoxide and nitrogen oxides causes serious harm to the environment, the long-time contact causes great harm to the health of human bodies, and the use of the polar solvents and the pyrolysis products thereof is gradually limited along with the gradual enhancement of environmental awareness of various countries. There is therefore a need for effective improvements in the current processes for preparing polyimide foams.
Chinese patent document CN105237766B discloses a method for preparing a flexible polyimide foam material with a regular cell structure, which relates to the preparation of a foaming material A, adding polyisocyanate into a carboxylic ester solution, stirring and reacting for 10-30 minutes under the nitrogen atmosphere, then putting the mixture into a vacuum box, vacuumizing until the vacuum degree reaches 0.1MPa, keeping the vacuum degree, and taking out the mixture after no more bubbles are generated in the mixture, thus obtaining the foaming material A. But the partial intermediate material is subjected to vacuum pre-reaction, and a polar solvent is still required to be used as a whole. For example, in the preparation of the carboxylic ester solution of the polybasic aromatic anhydride derivative, the polar solvent and the polybasic aromatic anhydride are added into a container, stirred and placed in an oil bath pot for heating, fatty alcohol is added into the container for esterification reaction when the temperature reaches 40-70 ℃, and a clear and transparent carboxylic ester solution is formed after the reaction is carried out for 2-3 hours. The carboxylate solution requires the presence of a polar solvent to prepare. It is difficult for the ordinary skilled person to derive from the patent document, and there is no motivation to consider how to use a polar solvent in order to carry out the solvent-free preparation of polyimide foam as a whole.
Chinese patent document CN104829835B discloses a method for preparing isocyanate group polyimide foam, which relates to the reaction of polyatomic aromatic anhydride and isocyanate to synthesize black material, specifically: and (2) sequentially and quickly adding the polar solvent, the polybasic aromatic anhydride and the isocyanate into a container at room temperature, connecting a nitrogen protection device, placing the container in an oil bath pot for heating, stirring, and obtaining the foamed black material after the polybasic aromatic anhydride reacts. Although the device is connected with a nitrogen protection device, the preparation of partial intermediate materials still needs to use a polar solvent on the whole. For example, the polybasic aromatic anhydride is heated and dissolved in a polar solvent to react with aliphatic alcohol to obtain the polybasic aromatic anhydride derivative solution. The solution of the polybasic aromatic anhydride derivative needs to be prepared by the participation of a polar solvent. It is still difficult for the ordinary skilled person to derive a suggestion from the patent document as to how to carry out the solvent-free preparation of polyimide foam as a whole, and there is no motivation to consider the technical problem of how to not use a polar solvent.
Disclosure of Invention
In view of the above, the inventor has made the present invention by making a creative effort. The invention aims to provide a solvent-free preparation method and a product of polyimide foam, and the method can be used for preparing the polyimide foam material with excellent performance and soft texture on the premise of not using a solvent, eliminating the problems of raw material cost and environmental pollution caused by the solvent in the traditional preparation technology of the polyimide foam, and providing a new technical thought for the preparation of the polyimide foam material.
The adopted technical scheme is as follows:
the invention relates to a solvent-free preparation method of polyimide foam, which comprises the following steps:
1) preparing a compound material: stirring a foaming agent, a surfactant and a catalyst for 0.5-2 hours at the temperature of 30-60 ℃, and uniformly mixing to obtain clear and transparent slurry; then, degassing the mixture for 1-5 hours under a vacuum condition, removing redundant air in the slurry to obtain a compound material, and sealing and storing the compound material for later use;
2) preparing polyimide intermediate slurry: firstly, sequentially adding polyisocyanate and polybasic aromatic anhydride into a reaction vessel at room temperature; then, a nitrogen protection device with a drying tube is connected, and nitrogen flows into the reaction container after being dried; then, placing the reaction vessel in an oil bath kettle at the temperature of 80-100 ℃, and starting a magnetic stirring device to react the polyisocyanate with the polybasic aromatic anhydride for 1-3 hours to obtain brown slurry; finally, removing the nitrogen protection device, keeping the heating temperature, connecting into a vacuum degassing device for degassing treatment for 1-3 hours, removing gas including carbon dioxide in the slurry, promoting the reaction of the polyisocyanate and the polybasic aromatic anhydride to move forwards, finally obtaining polyimide intermediate slurry, and sealing and storing for later use;
3) rapidly pouring the compound material prepared in the step 1) into the polyimide intermediate slurry prepared in the step 2 under the conditions of room temperature and normal pressure, and uniformly stirring to obtain foaming slurry;
4) pouring the foaming slurry into a foaming mould, immediately placing the foaming slurry into a vacuum oven heated to 80-100 ℃, simultaneously keeping the vacuum degree at 80-95kPa, then slowly and freely foaming and molding the foaming slurry in the mould, and keeping for 15-30 minutes to obtain a shaped polyimide foam intermediate;
5) and heating and curing the polyimide foam intermediate at the high temperature of 180-260 ℃ for 1-3 hours to finally prepare the solvent-free polyimide foam with soft texture.
Further, the material composition is as follows according to the parts by weight: 20-200 parts of foaming agent, 30-50 parts of surfactant, 2-15 parts of catalyst, 380 parts of polybasic aromatic anhydride and 400 parts of polyisocyanate.
Further, the polybasic aromatic acid anhydride is one or a mixture of more of pyromellitic dianhydride, 3',4,4' -benzophenone tetracarboxylic dianhydride, 3',4,4' -biphenyl tetracarboxylic dianhydride, 3',4,4' -diphenyl ether tetracarboxylic dianhydride and 3,3',4,4' -biphenyl sulfone tetracarboxylic dianhydride.
Further, the foaming agent is deionized water.
Further, the surfactant is a mixture of one or more of non-hydrolytic water-soluble polyether siloxane AK8805, DC193 and L580 and polyethylene oxide nonionic surfactants PEG-600, PEG-300, PEG-400, PEG-800 and PEG-1000.
Further, the catalyst is one or a mixture of more of triethanolamine, triethylene diamine, stannous octoate, dibutyltin dilaurate and Dabco 33-LV.
Further, the polyisocyanate is one or more of diphenylmethane diisocyanate (MDI), Toluene Diisocyanate (TDI) and polyphenyl polymethylene polyisocyanate (PAPI).
The solvent-free polyimide foam is prepared by the solvent-free preparation method of the polyimide foam.
Further, the density of the solvent-free polyimide foam is 25-36kg/m3The heat conductivity coefficient is 0.035-0.045W/(m.K), the limiting oxygen index is 37-43%, the glass transition temperature is 280-350 ℃, the tensile strength is 240-390kPa, and the texture is soft and can be bent and twisted for multiple times at 180 ℃ without cracking.
Compared with the existing preparation method of polyimide foam material, the preparation method has the following beneficial effects:
on the first hand, the intermediate of polyimide containing seven-membered ring structure is directly obtained by the pre-reaction of polyisocyanate and polybasic aromatic anhydride, and the reaction of anhydride and isocyanate is promoted to move forward by the vacuum-pumping degassing treatment, thus ensuring the polyimide content of the final product and the physical and chemical properties such as excellent flame retardance, heat resistance and the like.
In the second aspect, the polar solvent is not used in the whole preparation process, so that the production cost is reduced, the harm of the polar solvent to the environment and the human health is radically avoided, the industrial production and the wide application are facilitated, and the aim of the invention is achieved.
In the third aspect, the temperature and the vacuum degree of the vacuum oven are strictly controlled in a mode of reducing the viscosity of the slurry in a high-temperature environment and promoting the expansion of nucleation sites by vacuum assistance, so that the high foaming ratio and the low material density are effectively ensured, and the final product has good heat insulation performance.
Compared with CN105237766B and CN104829835B, the invention has the following beneficial effects:
the invention relates to the vacuum condition, so that the polar solvent is not used in the whole preparation process, and the use of the polar solvent is avoided from the root of the product preparation, for example, in the steps 1), 2) and 4).
Drawings
FIG. 1 is a digital photograph of a sample of solvent-free polyimide foam prepared in example 1.
FIG. 2 is a scanning electron micrograph of the solvent-free polyimide foam prepared in example 2.
Detailed Description
The present invention is described in detail below with reference to specific examples, but the use and purpose of these exemplary embodiments are merely to exemplify the present invention, and do not set forth any limitation on the actual scope of the present invention in any form, and the scope of the present invention is not limited thereto.
Example 1
At room temperature and normal pressure, 10 g of deionized water, 3 g of non-hydrolytic water-soluble polyether siloxane (AK8805) and 1 g of triethanolamine are added into a disposable plastic cup, and after being simply stirred by a glass rod, the disposable plastic cup is placed into a 45 ℃ water bath kettle to be continuously heated and stirred for 1 hour to obtain clear slurry. And then, placing the slurry in a vacuum oven for degassing treatment for 1.5 hours until no obvious bubbles exist in the slurry, thus obtaining a compound material, cooling to room temperature, and sealing and storing for later use. Simultaneously, 30 g of polyphenyl polymethylene polyisocyanate (PAPI) and 24 g of pyromellitic dianhydride are sequentially added into a three-neck flask at room temperature; then, a nitrogen protection device with a drying tube is connected, and nitrogen flows into the three-neck flask at the flow rate of 10ml/s after being dried; then, placing the reaction vessel in an oil bath kettle at 90 ℃, starting a magnetic stirring device, and reacting the reaction vessel and the magnetic stirring device for 2.5 hours to obtain brown slurry; and finally, removing the nitrogen protection device, keeping the heating temperature, connecting a vacuum pump for degassing for 2 hours, removing gases such as carbon dioxide in the slurry, promoting the reaction of the polyisocyanate and the polybasic aromatic anhydride to move forwards, finally obtaining polyimide intermediate slurry, and sealing and storing the polyimide intermediate slurry after the temperature is reduced to the room temperature for later use.
And (3) rapidly pouring the compound material into the polyimide intermediate slurry under the conditions of room temperature and normal pressure, and rapidly and uniformly stirring by using a high-speed stirring paddle to obtain the foaming material slurry. And then, pouring the foaming slurry into a foaming mold, immediately placing the foaming slurry into a vacuum oven heated to 100 ℃, simultaneously keeping the vacuum degree at 80kPa, then slowly and freely foaming and molding the foaming slurry in the mold, and keeping for 25 minutes to obtain a shaped polyimide foam intermediate. The obtained foam intermediate is heated and cured for 2 hours at a high temperature of 240 ℃ in a blast oven, and finally the solvent-free polyimide foam with soft texture is prepared.
Referring to fig. 1, fig. 1 is a digital photograph of a sample of solvent-free polyimide foam prepared in this example.
The density of the prepared solvent-free polyimide foam is 32kg/m3The thermal conductivity coefficient is 0.041W/(m.K), the limiting oxygen index is 41%, the glass transition temperature is 310 ℃, the tensile strength is 279kPa, and the texture is soft and can be bent and twisted for multiple times at 180 degrees without cracking.
Example 2
Under the condition of room temperature and normal pressure, a mixture prepared by 15 g of deionized water, 3 g of polyoxyethylene nonionic surfactant (PEG-600), 1 g of triethanolamine and Dabco33-LV according to the mass ratio of 2:1 is added into a disposable plastic cup, the mixture is simply stirred by a glass rod, and then the mixture is placed into a 45 ℃ water bath kettle to be continuously heated and stirred for 1 hour to obtain clear slurry. And then, placing the slurry in a vacuum oven for degassing treatment for 1 hour until no obvious bubbles exist in the slurry, thus obtaining a compound material, cooling to room temperature, and sealing and storing for later use. Simultaneously, 30 g of polyphenyl polymethylene polyisocyanate (PAPI) and 24 g of pyromellitic dianhydride are sequentially added into a three-neck flask at room temperature; then, a nitrogen protection device with a drying tube is connected, and nitrogen flows into the three-neck flask at the flow rate of 10ml/s after being dried; then, placing the reaction vessel in an oil bath kettle at 90 ℃, starting a magnetic stirring device, and reacting the reaction vessel and the magnetic stirring device for 3 hours to obtain brown slurry; and finally, removing the nitrogen protection device, keeping the heating temperature, connecting a vacuum pump for degassing for 3 hours, removing gases such as carbon dioxide in the slurry, promoting the reaction of the polyisocyanate and the polybasic aromatic anhydride to move forwards, finally obtaining polyimide intermediate slurry, and sealing and storing the polyimide intermediate slurry after the temperature is reduced to room temperature for later use.
And (3) rapidly pouring the compound material into the polyimide intermediate slurry under the conditions of room temperature and normal pressure, and rapidly and uniformly stirring by using a high-speed stirring paddle to obtain the foaming material slurry. And then, pouring the foaming slurry into a foaming mold, immediately placing the foaming slurry into a vacuum oven heated to 100 ℃, simultaneously keeping the vacuum degree at 95kPa, then slowly and freely foaming and molding the foaming slurry in the mold, and keeping for 30 minutes to obtain a shaped polyimide foam intermediate. The obtained foam intermediate is heated and cured for 2 hours in a blast oven at the high temperature of 260 ℃, and finally the solvent-free polyimide foam with soft texture is prepared.
Referring to fig. 2, fig. 2 is a scanning electron micrograph of the solvent-free polyimide foam prepared in this example.
The density of the prepared solvent-free polyimide foam is 25kg/m3The heat conductivity coefficient is 0.036W/(m.K), the limiting oxygen index is 39%, the glass transition temperature is 302 ℃, the tensile strength is 249kPa, and the texture is soft and can be bent and twisted for multiple times at 180 degrees without cracking.
Example 3
Under the condition of room temperature and normal pressure, a mixture prepared by 10 g of deionized water, 3 g of non-hydrolytic water-soluble polyether siloxane (AK8805) and 1.5 g of triethanolamine, Dabco33-LV and dibutyltin dilaurate according to the mass ratio of 4:2:1 is added into a disposable plastic cup, the mixture is simply stirred by a glass rod, and then the mixture is placed into a 45 ℃ water bath kettle to be continuously heated and stirred for 1 hour to obtain clear slurry. And then, placing the slurry in a vacuum oven for degassing treatment for 1 hour until no obvious bubbles exist in the slurry, thus obtaining a compound material, cooling to room temperature, and sealing and storing for later use. Simultaneously, 30 g of polyphenyl polymethylene polyisocyanate (PAPI) and 35 g of 3,3',4,4' -benzophenone tetracarboxylic dianhydride are sequentially added into a three-neck flask at room temperature; then, a nitrogen protection device with a drying tube is connected, and nitrogen flows into the three-neck flask at the flow rate of 7ml/s after being dried; then, placing the reaction vessel in an oil bath kettle at 100 ℃, starting a magnetic stirring device, and reacting the reaction vessel and the magnetic stirring device for 3 hours to obtain brown slurry; and finally, removing the nitrogen protection device, keeping the heating temperature, connecting a vacuum pump for degassing for 3 hours, removing gases such as carbon dioxide in the slurry, promoting the reaction of the polyisocyanate and the polybasic aromatic anhydride to move forwards, finally obtaining polyimide intermediate slurry, and sealing and storing the polyimide intermediate slurry after the temperature is reduced to room temperature for later use.
And (3) rapidly pouring the compound material into the polyimide intermediate slurry under the conditions of room temperature and normal pressure, and rapidly and uniformly stirring by using a high-speed stirring paddle to obtain the foaming material slurry. And then, pouring the foaming slurry into a foaming mold, immediately placing the foaming slurry into a vacuum oven heated to 100 ℃, simultaneously keeping the vacuum degree at 95kPa, then slowly and freely foaming and molding the foaming slurry in the mold, and keeping for 30 minutes to obtain a shaped polyimide foam intermediate. The obtained foam intermediate is heated and cured for 2 hours in a blast oven at the high temperature of 260 ℃, and finally the solvent-free polyimide foam with soft texture is prepared.
The density of the prepared solvent-free polyimide foam is 34kg/m3The thermal conductivity coefficient is 0.036W/(m.K), the limiting oxygen index is 42%, the glass transition temperature is 317 ℃, the tensile strength is 337kPa, and the texture is soft and can be bent and twisted for multiple times at 180 degrees without cracking.
The above-listed detailed description is only a specific description of a possible embodiment of the present invention, and they are not intended to limit the scope of the present invention, and equivalent embodiments or modifications made without departing from the technical spirit of the present invention should be included in the scope of the present invention.
Claims (9)
1. A solvent-free preparation method of polyimide foam is characterized by comprising the following steps:
1) preparing a compound material: stirring a foaming agent, a surfactant and a catalyst for 0.5-2 hours at the temperature of 30-60 ℃, and uniformly mixing to obtain clear and transparent slurry; then, degassing the mixture for 1-5 hours under a vacuum condition, removing redundant air in the slurry to obtain a compound material, and sealing and storing the compound material for later use;
2) preparing polyimide intermediate slurry: firstly, sequentially adding polyisocyanate and polybasic aromatic anhydride into a reaction vessel at room temperature; then, a nitrogen protection device with a drying tube is connected, and nitrogen flows into the reaction container after being dried; then, placing the reaction vessel in an oil bath kettle at the temperature of 80-100 ℃, and starting a magnetic stirring device to react the polyisocyanate with the polybasic aromatic anhydride for 1-3 hours to obtain brown slurry; finally, removing the nitrogen protection device, keeping the heating temperature, connecting into a vacuum degassing device for degassing treatment for 1-3 hours, removing gas including carbon dioxide in the slurry, promoting the reaction of the polyisocyanate and the polybasic aromatic anhydride to move forwards, finally obtaining polyimide intermediate slurry, and sealing and storing for later use;
3) rapidly pouring the compound material prepared in the step 1) into the polyimide intermediate slurry prepared in the step 2 under the conditions of room temperature and normal pressure, and uniformly stirring to obtain foaming slurry;
4) pouring the foaming slurry into a foaming mould, immediately placing the foaming slurry into a vacuum oven heated to 80-100 ℃, simultaneously keeping the vacuum degree at 80-95kPa, then slowly and freely foaming and molding the foaming slurry in the mould, and keeping for 15-30 minutes to obtain a shaped polyimide foam intermediate;
5) and heating and curing the polyimide foam intermediate at the high temperature of 180-260 ℃ for 1-3 hours to finally prepare the solvent-free polyimide foam with soft texture.
2. The solvent-free preparation method of polyimide foam according to claim 1, characterized in that: the material composition is as follows according to the parts by weight: 20-200 parts of foaming agent, 30-50 parts of surfactant, 2-15 parts of catalyst, 380 parts of polybasic aromatic anhydride and 400 parts of polyisocyanate.
3. The solvent-free preparation method of polyimide foam according to claim 1, characterized in that: the polybasic aromatic acid anhydride is one or a mixture of more than one of pyromellitic dianhydride, 3',4,4' -benzophenone tetracarboxylic dianhydride, 3',4,4' -biphenyl tetracarboxylic dianhydride, 3',4,4' -diphenyl ether tetracarboxylic dianhydride and 3,3',4,4' -biphenyl sulfone tetracarboxylic dianhydride.
4. The solvent-free preparation method of polyimide foam according to claim 1, characterized in that: the foaming agent is deionized water.
5. The solvent-free preparation method of polyimide foam according to claim 1, characterized in that: the surfactant is a mixture of one or more of non-hydrolytic water-soluble polyether siloxane AK8805, DC193 and L580 and polyoxyethylene nonionic surfactants PEG-600, PEG-300, PEG-400, PEG-800 and PEG-1000.
6. The solvent-free preparation method of polyimide foam according to claim 1, characterized in that: the catalyst is one or a mixture of triethanolamine, triethylene diamine, stannous octoate, dibutyltin dilaurate and Dabco 33-LV.
7. The solvent-free preparation method of polyimide foam according to claim 1, characterized in that: the polyisocyanate is one or a mixture of diphenylmethane diisocyanate, toluene diisocyanate and polyphenyl polymethylene polyisocyanate.
8. A solvent-free polyimide foam produced by the solvent-free production method for a polyimide foam according to any one of claims 1 to 7.
9. The solvent-free polyimide foam according to claim 8, wherein: the solvent-free polyimideThe density of the amine foam is 25-36kg/m3The heat conductivity coefficient is 0.035-0.045W/(m.K), the limiting oxygen index is 37-43%, the glass transition temperature is 280-350 ℃, the tensile strength is 240-390kPa, and the texture is soft and can be bent and twisted for multiple times at 180 ℃ without cracking.
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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 |
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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 |
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