CN113372610A - Preparation method of polyimide aerogel glass - Google Patents
Preparation method of polyimide aerogel glass Download PDFInfo
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- CN113372610A CN113372610A CN202110888654.2A CN202110888654A CN113372610A CN 113372610 A CN113372610 A CN 113372610A CN 202110888654 A CN202110888654 A CN 202110888654A CN 113372610 A CN113372610 A CN 113372610A
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- wet gel
- aerogel glass
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- 239000004642 Polyimide Substances 0.000 title claims abstract description 40
- 229920001721 polyimide Polymers 0.000 title claims abstract description 40
- 239000011521 glass Substances 0.000 title claims abstract description 38
- 239000004964 aerogel Substances 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 238000001035 drying Methods 0.000 claims abstract description 44
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 33
- 239000011240 wet gel Substances 0.000 claims abstract description 30
- 229920005575 poly(amic acid) Polymers 0.000 claims abstract description 18
- 239000002243 precursor Substances 0.000 claims abstract description 16
- 238000003756 stirring Methods 0.000 claims abstract description 11
- 239000002904 solvent Substances 0.000 claims abstract description 10
- GTDPSWPPOUPBNX-UHFFFAOYSA-N ac1mqpva Chemical compound CC12C(=O)OC(=O)C1(C)C1(C)C2(C)C(=O)OC1=O GTDPSWPPOUPBNX-UHFFFAOYSA-N 0.000 claims abstract description 8
- 150000004985 diamines Chemical class 0.000 claims abstract description 8
- 230000032683 aging Effects 0.000 claims abstract description 6
- 238000002791 soaking Methods 0.000 claims abstract description 6
- 239000003054 catalyst Substances 0.000 claims abstract description 5
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 5
- 239000012024 dehydrating agents Substances 0.000 claims abstract description 5
- WFDIJRYMOXRFFG-UHFFFAOYSA-N Acetic anhydride Chemical group CC(=O)OC(C)=O WFDIJRYMOXRFFG-UHFFFAOYSA-N 0.000 claims description 27
- 239000000243 solution Substances 0.000 claims description 21
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 claims description 18
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 12
- VLDPXPPHXDGHEW-UHFFFAOYSA-N 1-chloro-2-dichlorophosphoryloxybenzene Chemical compound ClC1=CC=CC=C1OP(Cl)(Cl)=O VLDPXPPHXDGHEW-UHFFFAOYSA-N 0.000 claims description 9
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 claims description 9
- MBYLVOKEDDQJDY-UHFFFAOYSA-N tris(2-aminoethyl)amine Chemical compound NCCN(CCN)CCN MBYLVOKEDDQJDY-UHFFFAOYSA-N 0.000 claims description 9
- 230000000694 effects Effects 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 8
- QYIMZXITLDTULQ-UHFFFAOYSA-N 4-(4-amino-2-methylphenyl)-3-methylaniline Chemical group CC1=CC(N)=CC=C1C1=CC=C(N)C=C1C QYIMZXITLDTULQ-UHFFFAOYSA-N 0.000 claims description 7
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 6
- 239000012530 fluid Substances 0.000 claims description 5
- 238000005086 pumping Methods 0.000 claims description 5
- 238000000352 supercritical drying Methods 0.000 claims description 5
- 239000000499 gel Substances 0.000 claims description 4
- AWJUIBRHMBBTKR-UHFFFAOYSA-N isoquinoline Chemical compound C1=NC=CC2=CC=CC=C21 AWJUIBRHMBBTKR-UHFFFAOYSA-N 0.000 claims description 4
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 3
- PAPDRIKTCIYHFI-UHFFFAOYSA-N 4-[3,5-bis(4-aminophenoxy)phenoxy]aniline Chemical compound C1=CC(N)=CC=C1OC1=CC(OC=2C=CC(N)=CC=2)=CC(OC=2C=CC(N)=CC=2)=C1 PAPDRIKTCIYHFI-UHFFFAOYSA-N 0.000 claims description 2
- 150000003512 tertiary amines Chemical class 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 4
- 150000008064 anhydrides Chemical class 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 7
- 238000002834 transmittance Methods 0.000 abstract description 4
- 238000010924 continuous production Methods 0.000 abstract description 2
- 238000011049 filling Methods 0.000 abstract description 2
- LGRFSURHDFAFJT-UHFFFAOYSA-N Phthalic anhydride Natural products C1=CC=C2C(=O)OC(=O)C2=C1 LGRFSURHDFAFJT-UHFFFAOYSA-N 0.000 description 2
- 239000004965 Silica aerogel Substances 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- JHIWVOJDXOSYLW-UHFFFAOYSA-N butyl 2,2-difluorocyclopropane-1-carboxylate Chemical compound CCCCOC(=O)C1CC1(F)F JHIWVOJDXOSYLW-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Classifications
-
- 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
- C08J9/28—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof by elimination of a liquid phase from a macromolecular composition or article, e.g. drying of coagulum
-
- 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
- C08G73/1007—Preparatory processes from tetracarboxylic acids or derivatives and diamines
-
- 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
- C08G73/1039—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors comprising halogen-containing substituents
-
- 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
- C08G73/1067—Wholly aromatic polyimides, i.e. having both tetracarboxylic and diamino moieties aromatically bound
-
- 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
- C08J2201/00—Foams characterised by the foaming process
- C08J2201/04—Foams characterised by the foaming process characterised by the elimination of a liquid or solid component, e.g. precipitation, leaching out, evaporation
- C08J2201/05—Elimination by evaporation or heat degradation of a liquid phase
- C08J2201/0502—Elimination by evaporation or heat degradation of a liquid phase the liquid phase being organic
-
- 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
- C08J2205/00—Foams characterised by their properties
- C08J2205/02—Foams characterised by their properties the finished foam itself being a gel or a gel being temporarily formed when processing the foamable composition
- C08J2205/026—Aerogel, i.e. a supercritically dried gel
-
- 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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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Macromolecular Compounds Obtained By Forming Nitrogen-Containing Linkages In General (AREA)
Abstract
The invention discloses a preparation method of polyimide aerogel glass, which comprises the following steps: (1) preparing a polyamic acid solution: sequentially adding a dianhydride precursor and a diamine precursor into a solvent, and stirring until the dianhydride precursor and the diamine precursor are completely dissolved to form a polyamic acid solution system; (2) preparing a polyimide wet gel: adding a cross-linking agent, a dehydrating agent and a catalyst into the polyamic acid solution, stirring, and standing at normal temperature until the solution is gelled; (3) aging of the polyimide wet gel: soaking the prepared wet gel in 99% industrial methanol for 48 hours; (4) and (3) drying: and drying the aged wet gel to obtain the polyimide aerogel glass. The polyimide aerogel glass prepared by the invention has better mechanical strength, can be used for preparing a whole aerogel glass filling layer, is simple in preparation method and controllable in process, can realize continuous production, and has good light transmittance while ensuring the heat-insulating property.
Description
Technical Field
The invention belongs to the technical field of aerogel glass preparation, and particularly relates to a preparation method of polyimide aerogel glass.
Background
Aerogel glass utilizes the aerogel to fill the novel building material who makes between two transparent glass boards, and the structure is similar with traditional double glazing, but adiabatic effect is several times higher than ordinary double glazing, and has the effect of making an uproar of falling, can effectively compensate not enough on ordinary glass window uses. Silica aerogel particle-filled glass is currently commonly used because silica aerogel has high brittleness, making it difficult to prepare in bulk, and monolithic aerogels have better light transmittance and lower heat transfer coefficient. Therefore, there is an urgent need for improvements in the preparation of current aerogel glasses to achieve better performance of aerogel glasses.
Disclosure of Invention
In order to solve the above problems, the present invention provides a method for preparing a polyimide aerogel glass.
A preparation method of polyimide aerogel glass comprises the following steps:
(1) preparing a polyamic acid solution: sequentially adding a dianhydride precursor and a diamine precursor into a solvent, and stirring for 2min until the dianhydride precursor and the diamine precursor are completely dissolved to form a polyamic acid solution system, wherein the dianhydride precursor comprises one or two mixtures of pyromellitic dianhydride and 4,4 '-hexafluoroisopropyl phthalic anhydride (6FDA), the diamine precursor is 4, 4' -diamino-2, 2 '-dimethyl-1, 1' -biphenyl, and the solvent is one or two mixtures of N, N-dimethylformamide and N-methylpyrrolidone;
(2) preparing a polyimide wet gel: adding a cross-linking agent, a dehydrating agent and a catalyst into a polyamic acid solution, stirring for 5min, standing at normal temperature until the solution is gelled, wherein the cross-linking agent is one or a mixture of two of tris (2-aminoethyl) amine and 1,3, 5-tris (4-aminophenoxy) benzene, the dehydrating agent is acetic anhydride, and the catalyst is one or more of tertiary amines such as pyridine, isoquinoline or triethylamine;
(3) aging of the polyimide wet gel: soaking the prepared wet gel in 99% industrial methanol for 48 hours, and replacing the methanol every 8 hours;
(4) and (3) drying: drying the aged wet gel to obtain the polyimide aerogel glass, wherein the drying is to put the aged wet gel into a drying kettle, and then to put the aged wet gel into the drying kettleCO2Pumping into a drying kettle by a pump, and keeping CO in the drying kettle2Is in a supercritical state, using supercritical fluid CO2The solvent in the alcogel is replaced by the dissolving capacity and the ultra-low surface tension of the CO, so that the drying effect is achieved2The supercritical state temperature of (A) is 45-55 deg.C, the pressure is 10-16MPa, and CO is2The flow rate passing through the supercritical drying kettle is 1500-3500kg/h, and the drying time is 4-12 h.
In order to enhance the mechanical strength of the polyimide aerogel glass, the ratio of the pyromellitic dianhydride, the 4,4 ' -diamino-2, 2 ' -dimethyl-1, 1 ' -biphenyl, the tris (2-aminoethyl) amine, the pyridine and the acetic anhydride is 1:0.97:0.02:8: 8.
Compared with the prior art, the preparation method of the polyimide aerogel glass has the beneficial effects that: 1. the polyimide aerogel glass prepared by the invention has better mechanical strength, can be used for preparing a whole aerogel glass filling layer, is simple in preparation method and controllable in process, and can realize continuous production; 2. the density of the polyimide aerogel glass prepared by the invention is 0.05-0.09g/cm3The heat conductivity coefficient is 0.015-0.03W/m.K, the visible light transmittance is 65% -80%, and the whole polyimide aerogel glass has good light transmittance while ensuring the heat insulation performance.
Detailed Description
The following description of the embodiments of the present invention is provided for illustrative purposes, and other advantages and effects of the present invention will become apparent to those skilled in the art from the present disclosure.
It is to be noted that the term "comprises," "comprising," or any other variation thereof is intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
Example 1
A preparation method of polyimide aerogel glass comprises the following steps:
(1) preparing a polyamic acid solution: sequentially adding pyromellitic dianhydride and 4,4 ' -diamino-2, 2 ' -dimethyl-1, 1 ' -biphenyl into N, N-dimethylformamide, and stirring for 2min until completely dissolving to form a polyamic acid solution system;
(2) preparing a polyimide wet gel: adding tris (2-aminoethyl) amine, acetic anhydride and pyridine into the polyamic acid solution, stirring for 5min, and standing at normal temperature until the solution gels;
(3) aging of the polyimide wet gel: soaking the prepared wet gel in 99% industrial methanol for 48 hours, and replacing the methanol every 8 hours;
(4) and (3) drying: drying the aged wet gel to obtain the polyimide aerogel glass, wherein the drying is to put the aged wet gel into a drying kettle and to add CO2Pumping into a drying kettle by a pump, and keeping CO in the drying kettle2Is in a supercritical state, using supercritical fluid CO2The solvent in the alcogel is replaced by the dissolving capacity and the ultra-low surface tension of the CO, so that the drying effect is achieved2The supercritical state temperature of (A) is 55 ℃, the pressure is 14MPa, and CO is2The flow rate through the supercritical drying kettle was 2500kg/h, and the drying time was 5 h.
In order to enhance the mechanical strength of the polyimide aerogel glass, the ratio of the pyromellitic dianhydride, the 4,4 ' -diamino-2, 2 ' -dimethyl-1, 1 ' -biphenyl, the tris (2-aminoethyl) amine, the pyridine and the acetic anhydride is 1:0.97:0.02:8: 8.
Example 2
A preparation method of polyimide aerogel glass comprises the following steps:
(1) preparing a polyamic acid solution: sequentially adding pyromellitic dianhydride and 4,4 ' -diamino-2, 2 ' -dimethyl-1, 1 ' -biphenyl into N-methyl pyrrolidone, and stirring for 2min until completely dissolving to form a polyamic acid solution system;
(2) preparing a polyimide wet gel: adding tris (2-aminoethyl) amine, acetic anhydride and pyridine into the polyamic acid solution, stirring for 5min, and standing at normal temperature until the solution gels;
(3) aging of the polyimide wet gel: soaking the prepared wet gel in 99% industrial methanol for 48 hours, and replacing the methanol every 8 hours;
(4) and (3) drying: drying the aged wet gel to obtain the polyimide aerogel glass, wherein the drying is to put the aged wet gel into a drying kettle and to add CO2Pumping into a drying kettle by a pump, and keeping CO in the drying kettle2Is in a supercritical state, using supercritical fluid CO2The solvent in the alcogel is replaced by the dissolving capacity and the ultra-low surface tension of the CO, so that the drying effect is achieved2The supercritical state temperature of (A) is 55 ℃, the pressure is 14MPa, and CO is2The flow rate through the supercritical drying kettle was 2500kg/h, and the drying time was 5 h.
In order to enhance the mechanical strength of the polyimide aerogel glass, the ratio of the pyromellitic dianhydride, the 4,4 ' -diamino-2, 2 ' -dimethyl-1, 1 ' -biphenyl, the tris (2-aminoethyl) amine, the pyridine and the acetic anhydride is 1:0.97:0.02:8: 8.
Example 3
A preparation method of polyimide aerogel glass comprises the following steps:
(1) preparing a polyamic acid solution: mixing pyromellitic dianhydride and 4,4 '-hexafluoroisopropyl phthalic anhydride (6FDA), and then sequentially adding 4' -diamino-2, 2 '-dimethyl-1, 1' -biphenyl into N, N-dimethylformamide to be stirred for 2min until the mixture is completely dissolved, so as to form a polyamic acid solution system;
(2) preparing a polyimide wet gel: adding tris (2-aminoethyl) amine, acetic anhydride and pyridine into the polyamic acid solution, stirring for 5min, and standing at normal temperature until the solution gels;
(3) aging of the polyimide wet gel: soaking the prepared wet gel in 99% industrial methanol for 48 hours, and replacing the methanol every 8 hours;
(4) and (3) drying: drying the aged wet gel to obtain the polyimide aerogel glass, wherein the drying is to put the aged wet gel into a drying kettle and to add CO2Pumping into a drying kettle by a pump, and keeping CO in the drying kettle2At a temperature and a pressure ofSupercritical state, using supercritical fluid CO2The solvent in the alcogel is replaced by the dissolving capacity and the ultra-low surface tension of the CO, so that the drying effect is achieved2The supercritical state temperature of (A) is 55 ℃, the pressure is 14MPa, and CO is2The flow rate through the supercritical drying kettle was 2500kg/h, and the drying time was 5 h.
The scope of the present invention is not limited to the technical solutions disclosed in the embodiments, and any modifications, equivalent substitutions, improvements, etc. made to the above embodiments according to the technical spirit of the present invention fall within the scope of the present invention.
Claims (5)
1. The preparation method of the polyimide aerogel glass is characterized by comprising the following steps of:
(1) preparing a polyamic acid solution: sequentially adding a dianhydride precursor and a diamine precursor into a solvent, and stirring for 2min until the dianhydride precursor and the diamine precursor are completely dissolved to form a polyamic acid solution system;
(2) preparing a polyimide wet gel: adding a cross-linking agent, a dehydrating agent and a catalyst into the polyamic acid solution, stirring for 5min, and standing at normal temperature until the solution gels;
(3) aging of the polyimide wet gel: soaking the prepared wet gel in 99% industrial methanol for 48 hours, and replacing the methanol every 8 hours;
(4) and (3) drying: and drying the aged wet gel to obtain the polyimide aerogel glass.
2. The method for producing a polyimide aerogel glass according to claim 1, wherein the dianhydride precursor comprises one or a mixture of pyromellitic dianhydride and 4,4 '-hexafluoroisopropylphthalic anhydride (6FDA), the diamine precursor is 4, 4' -diamino-2, 2 '-dimethyl-1, 1' -biphenyl, the solvent is one or a mixture of N, N-dimethylformamide and N-methylpyrrolidone, the crosslinking agent is one or a mixture of tris (2-aminoethyl) amine and 1,3, 5-tris (4-aminophenoxy) benzene, the dehydrating agent is acetic anhydride, and the catalyst is one or a mixture of pyridine, isoquinoline or triethylamine and other tertiary amines.
3. The method for producing a polyimide aerogel glass according to claim 2, wherein the ratio of pyromellitic dianhydride, 4 ' -diamino-2, 2 ' -dimethyl-1, 1 ' -biphenyl, tris (2-aminoethyl) amine, pyridine and acetic anhydride is 1:0.97:0.02:8: 8.
4. The method for producing the polyimide aerogel glass according to claim 2 or 3, wherein the drying step comprises placing the aged wet gel in a drying vessel, and introducing CO into the drying vessel2Pumping into a drying kettle by a pump, and keeping CO in the drying kettle2Is in a supercritical state, using supercritical fluid CO2The solvent in the alcogel is replaced by the dissolving capacity and the ultra-low surface tension, thereby achieving the drying effect.
5. The method for producing the polyimide aerogel glass according to claim 4, wherein the CO is present in the glass2The supercritical state temperature of (A) is 45-55 deg.C, the pressure is 10-16MPa, and CO is2The flow rate passing through the supercritical drying kettle is 1500-3500kg/h, and the drying time is 4-12 h.
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| CN202110888654.2A CN113372610A (en) | 2021-08-04 | 2021-08-04 | Preparation method of polyimide aerogel glass |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US9309369B1 (en) * | 2009-09-30 | 2016-04-12 | The United States Of America, As Represented By The Administrator Of The National Aeronautics And Space Administration | Polyimide aerogels with three-dimensional cross-linked structure |
| CN106746684A (en) * | 2016-12-26 | 2017-05-31 | 李光武 | A kind of glass and its application |
| CN110903511A (en) * | 2019-11-29 | 2020-03-24 | 无锡创彩光学材料有限公司 | Flexible flame-retardant polyimide aerogel and preparation method thereof |
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2021
- 2021-08-04 CN CN202110888654.2A patent/CN113372610A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US9309369B1 (en) * | 2009-09-30 | 2016-04-12 | The United States Of America, As Represented By The Administrator Of The National Aeronautics And Space Administration | Polyimide aerogels with three-dimensional cross-linked structure |
| CN106746684A (en) * | 2016-12-26 | 2017-05-31 | 李光武 | A kind of glass and its application |
| CN110903511A (en) * | 2019-11-29 | 2020-03-24 | 无锡创彩光学材料有限公司 | Flexible flame-retardant polyimide aerogel and preparation method thereof |
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