CN103214688B - Polyamide-imide foam and its preparation method - Google Patents
Polyamide-imide foam and its preparation method Download PDFInfo
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Abstract
The present invention provides the preparation method of a kind of Polyamide-imide foam, comprising: trimellitic acid 1,2-anhydride, whipping agent, catalyzer and tensio-active agent are mixed in a solvent, obtains the first solution; First solution and polyisocyanate solution mixed, stirs, foam, obtain foam intermediate; Foam intermediate imidization is obtained Polyamide-imide foam. The present invention adopts trimellitic acid 1,2-anhydride and polyisocyanates polymerization reaction take place, produces gas simultaneously and polymer foaming is shaped. The present invention adopts trimellitic acid 1,2-anhydride and polyisocyanates polyreaction, and the Polyamide-imide foam thermostability height obtained and density are low; The present invention's reaction is without the need to complicated preparation conditions such as high temperature, and technique is simple.
Description
Technical field
The present invention relates to technical field of polymer materials, especially relate to a kind of Polyamide-imide foam and its preparation method.
Background technology
Polyamidoimide is simultaneously containing a base polymer of heat-resisting imide ring and flexible amide group in a class backbone structure. Polyamidoimide has the feature performance benefit of polymeric amide and polyimide concurrently, has excellent thermotolerance, dielectricity, mechanical property and chemical stability. Although the amide group thermotolerance contained in the main chain of polyamidoimide relatively polyimide decrease, but amide group can make molecule chain rigidity reduce, and solubility is improved, thus improves rheological property and the processing characteristics of polymkeric substance. Meanwhile, polyamidoimide has the electro permanent magnetic under excellent anti-yaw damper performance and high temperature, high frequency condition, therefore can make the ablator of aircraft, magnetic-permeable material and structured material. Metal is had good adhesiveproperties by polyamidoimide, is applicable to make wire enamel, impregnating varnish, film, laminated plate material, coating and tackiness agent. In addition, polyamidoimide can also prepare moulding compound, prepares the structural parts such as various gear, roller, bearing through mold pressing.
Except above purposes, a kind of important use of polyamidoimide is processed into foam materials, compared to conventional foam such as urethane, polyethylene, polystyrene, Polyamide-imide foam has excellent flame retardant resistance, difficult combustion, low cigarette, without obnoxious flavour release, radiation hardness, resistance to chemical attack and can use under the high temperature conditions. Prior art discloses the preparation method of multiple Polyamide-imide foam, if US Patent No. 4604409 is by after two acid anhydrides of fragrance and the reaction of fatty hexanolactam, add isocyanate reaction, obtain the polyamide-imide foam materials that main chain contains six carbocyclic aliphatic chains. But this polymer chain introduces a large amount of fat chain structures, the poor heat stability of the foam materials of acquisition.
US Patent No. 4990543 discloses the preparation method of a kind of Polyamide-imide foam: vulcabond and trimellitic acid 1,2-anhydride, the polymerization of ketone acid anhydride obtain oligopolymer, when strict control carbon dioxide releasing amount, and the precursor powder of preparation foaming. Then 230 �� of C foaming. But this technique precursor powder complicated process of preparation, blowing temperature height.
US Patent No. 4960549 discloses the method utilizing extrusion equipment to prepare polyamide-imide foam. But, the comparatively complicated and obtained foam densities of this foam process equipment is up to 300g/cm3, the soft foam materials compared with low density cannot be obtained.
Summary of the invention
In view of this, the technical problem to be solved in the present invention is to provide a kind of Polyamide-imide foam, and the technique of Polyamide-imide foam provided by the invention is simple, density is low and thermostability height.
The present invention provides the preparation method of a kind of Polyamide-imide foam, comprising:
A) trimellitic acid 1,2-anhydride, whipping agent, catalyzer and tensio-active agent are mixed in a solvent, obtain the first solution;
B) the first solution and polyisocyanate solution mixed, stir, foam, obtain foam intermediate;
C) foam intermediate imidization is obtained Polyamide-imide foam.
Preferably, in described steps A, solvent is selected from N-Methyl pyrrolidone, the one in N, N '-N,N-DIMETHYLACETAMIDE, N, N '-dimethyl formamide;
One or more that in described steps A, whipping agent is selected from water, methyl alcohol, ethanol, propyl alcohol, butanols, ethylene glycol, acetone, tetrahydrofuran (THF) and ethylene glycol monomethyl ether;
One or more that in described steps A, catalyzer is selected from trolamine, triethylene diamine, triethylenediamine, two (2-dimethylaminoethyl) ether, Dabco33-LV, DabcoCS90, Polycat41, stannous octoate, dibutyl tin laurate, mercaptan dioctyl tin and dibutyltin diacetate;
In described steps A, tensio-active agent is selected from low molecular poly, one or more in DC5598, DC193, DC195, DC197, DC198, KH550, AK168, L620 and L6900.
Preferably, in described first solution, the mass ratio of trimellitic acid 1,2-anhydride, solvent, whipping agent, catalyzer and tensio-active agent is (100): (100��300): (5��28): (0.02��10): (5��40).
Preferably, in described polyisocyanate solution, the mass ratio of polyisocyanates and solvent is 1:(1��3).
Preferably, in described step B, the mass ratio of the first solution and polyisocyanate solution is 1:(0.1��2).
Preferably, one or more that in described polyisocyanate solution, polyisocyanates is selected from polyphenyl polymethylene polyisocyanates, the different hydrogen acid ether of toluene two, diphenylmethanediisocyanate, isophorone diisocyanate, xylylene diisocyanate and tetramethylxylylene diisocyanate;
In described polyisocyanate solution, solvent is selected from N-Methyl pyrrolidone, the one in N, N '-N,N-DIMETHYLACETAMIDE, N, N '-dimethyl formamide.
Preferably, in described step B, churning time is 10��30s, and described whipping temp is 25 DEG C��30 DEG C.
Preferably, in described step B, the time of foaming is 1��5min, and described blowing temperature is 25 DEG C��30 DEG C.
Preferably, in described step C, imidization tool temperature is 50 DEG C��300 DEG C, and the time of imidization is 3��5h.
Present invention also offers a kind of Polyamide-imide foam, prepare by the preparation method described in technique scheme.
Compared with prior art, the preparation method of a kind of Polyamide-imide foam, comprising: trimellitic acid 1,2-anhydride, whipping agent, catalyzer and tensio-active agent are mixed in a solvent, obtains the first solution; First solution and polyisocyanate solution mixed, stirs, foam, obtain foam intermediate; Foam intermediate imidization is obtained Polyamide-imide foam. The present invention adopts trimellitic acid 1,2-anhydride and polyisocyanates polymerization reaction take place, produces gas simultaneously and polymer foaming is shaped. The present invention adopts trimellitic acid 1,2-anhydride and polyisocyanates polyreaction, and the Polyamide-imide foam thermostability height obtained and density are low; The present invention's reaction is without the need to complicated preparation conditions such as high temperature, and technique is simple. Experimental result shows, the apparent density of the Polyamide-imide foam that the present invention prepares is 10.9Kg/m3, glass transition temp is 280 DEG C, and 5% thermal weight loss temperature is 326 DEG C, and compressive strength is 0.07144MPa, and tensile strength is 0.1078MPa.
Embodiment
A preparation method for Polyamide-imide foam, comprising:
A) trimellitic acid 1,2-anhydride, whipping agent, catalyzer and tensio-active agent are mixed in a solvent, obtain the first solution;
B) the first solution and polyisocyanate solution mixed, stir, foam, obtain foam intermediate;
C) foam intermediate imidization is obtained Polyamide-imide foam.
First trimellitic acid 1,2-anhydride, whipping agent, catalyzer and tensio-active agent are mixed by the present invention in a solvent, obtain the first solution. The present invention for described hybrid mode and unrestricted, hybrid mode well known to those skilled in the art, it is preferable to be uniformly mixed, described in the temperature preferably 25 DEG C��30 DEG C that is uniformly mixed.
In the present invention, in described steps A, solvent is preferably selected from N-Methyl pyrrolidone, the one in N, N '-N,N-DIMETHYLACETAMIDE, N, N '-dimethyl formamide; More preferably N, N '-N,N-DIMETHYLACETAMIDE and N it is selected from, the one in N '-dimethyl formamide.
In the present invention, one or more that in described steps A, whipping agent is preferably selected from water, methyl alcohol, ethanol, propyl alcohol, butanols, ethylene glycol, acetone, tetrahydrofuran (THF) and ethylene glycol monomethyl ether; More preferably one or more being selected from water, methyl alcohol, ethanol, propyl alcohol, butanols, ethylene glycol, acetone; One or more being most preferably selected from water, methyl alcohol, ethanol, propyl alcohol.
In the present invention, one or more that in described steps A, catalyzer is preferably selected from trolamine, triethylene diamine, triethylenediamine, two (2-dimethylaminoethyl) ether, Dabco33-LV, DabcoCS90, Polycat41, stannous octoate, dibutyl tin laurate, mercaptan dioctyl tin and dibutyltin diacetate; More preferably one or more being selected from trolamine, triethylene diamine, stannous octoate, dibutyl tin laurate, mercaptan dioctyl tin and dibutyltin diacetate; One or more being most preferably selected from trolamine, stannous octoate, dibutyl tin laurate and dibutyltin diacetate.
In the present invention, in described steps A, tensio-active agent is preferably selected from low molecular poly, one or more in DC5598, DC193, DC195, DC197, DC198, KH550, AK168, L620 and L6900; More preferably polyoxyethylene glycol it is selected from, one or more in DC5598, DC193, DC195, DC197, DC198 and L620; Most preferably it is selected from polyoxyethylene glycol, one or more in DC193, DC195, DC197.
In the present invention, in described first solution, the mass ratio of trimellitic acid 1,2-anhydride, solvent, whipping agent, catalyzer and tensio-active agent is preferably (100): (100��300): (5��28): (0.02��10): (5��40); In described steps A, the mass ratio of trimellitic acid 1,2-anhydride, solvent, whipping agent, catalyzer and tensio-active agent is more preferably (100): (120��280): (8��25): (0.1��8): (8��35).
After obtaining the first solution, the first solution and polyisocyanate solution mixed, stirs, foam, obtain foam intermediate. It is specially and the first solution is added in polyisocyanate solution, be uniformly mixed, pour in mould, free foaming, obtain foam intermediate. Described churning time is preferably 10��30 seconds, and described whipping temp is preferably 25 DEG C��30 DEG C. After stirring, solution starts to turn white, CO2Gas starts to release. The time of described foaming is preferably 1��5min, it is more preferable to be 3��5min. Described blowing temperature is preferably 25 DEG C��30 DEG C.
In described first solution, the mass ratio of trimellitic acid 1,2-anhydride, solvent, whipping agent, catalyzer and tensio-active agent is preferably (100): (100��300): (5��28): (0.02��10): (5��40); In described steps A, the mass ratio of trimellitic acid 1,2-anhydride, solvent, whipping agent, catalyzer and tensio-active agent is more preferably (100): (120��280): (8��25): (0.1��8): (8��35). In described polyisocyanate solution, the mass ratio of polyisocyanates and solvent is preferably 1:(1��3). The mass ratio of above-mentioned first solution and polyisocyanate solution is preferably 1:(0.1��2).
In the present invention, one or more that in described polyisocyanate solution, polyisocyanates is preferably selected from polyphenyl polymethylene polyisocyanates, the different hydrogen acid ether of toluene two, diphenylmethanediisocyanate, isophorone diisocyanate, xylylene diisocyanate and tetramethylxylylene diisocyanate; More preferably one or more being selected from polyphenyl polymethylene polyisocyanates, the different hydrogen acid ether of toluene two, diphenylmethanediisocyanate and isophorone diisocyanate; One or more being most preferably selected from polyphenyl polymethylene polyisocyanates, diphenylmethanediisocyanate and isophorone diisocyanate.
In described polyisocyanate solution, solvent is preferably selected from N-Methyl pyrrolidone, the one in N, N '-N,N-DIMETHYLACETAMIDE, N, N '-dimethyl formamide, it is more preferable to be selected from N, N '-N,N-DIMETHYLACETAMIDE and N, the one in N '-dimethyl formamide.
In the present invention, in described first solution, solvent can be identical with solvent in polyisocyanate solution, it is also possible to different, and the present invention is also unrestricted to this.
After obtaining foam intermediate, foam intermediate imidization is obtained Polyamide-imide foam. Described imidization imidization temperature is preferably 50 DEG C��300 DEG C, and the time of imidization is preferably 3��5h. Described imidization is preferably slaking, except solvent and imidization three phases, is specially at the temperature of 50 DEG C��100 DEG C slaking 40min��80min; Except solvent 40min��90min at the temperature of 100 DEG C��200 DEG C; At 200 DEG C��300 DEG C imidization 1.5h��2.5h. After preferred imidization, cooling obtains Polyamide-imide foam. The present invention is also unrestricted for the described type of cooling, the type of cooling well known to those skilled in the art.
The present invention adopts trimellitic acid 1,2-anhydride and polyisocyanates polymerization reaction take place, produces gas simultaneously and polymer foaming is shaped. The present invention adopts trimellitic acid 1,2-anhydride and polyisocyanates polyreaction, and the Polyamide-imide foam thermostability height obtained and density are low; The present invention's reaction is without the need to complicated preparation conditions such as high temperature, and technique is simple.
The Polyamide-imide foam that the present invention is preferably prepared by the present invention in the following ways carries out performance test, and detailed process is as follows:
The present invention adopts dynamic thermomechanical analysis apparatus, in a compressed mode, is measured by the second-order transition temperature of the Polyamide-imide foam obtained with the temperature rise rate of 5 �� of C/min;
The Polyamide-imide foam square-cut block that the present invention will obtain, measures its volume and quality thus calculates its apparent density;
The present invention adopts thermal weight loss TGA analysis tester, at N2Under condition, with the temperature rise rate of 10 �� of C/min, the thermal weight loss situation of prepared foam is measured; The second-order transition temperature of Polyamide-imide foam, apparent density, 5% thermal weight loss temperature,
In order to the present invention is described further, below in conjunction with embodiment, Polyamide-imide foam provided by the invention and its preparation method are described in detail.
Embodiment 1
148g trimellitic acid 1,2-anhydride, 10g methyl alcohol, 12g deionized water, 17gDC-193,6.5g polyoxyethylene glycol, 0.1g trolamine and 0.1g dibutyl tin laurate are joined 120gN respectively, in N '-dimethyl formamide (DMF) solution, stirring at room temperature is uniformly dissolved, and obtains the first solution.
Embodiment 2
100g polyphenyl polymethylene polyisocyanates is dissolved in 100gN, in N '-dimethyl formamide, obtains the 2nd solution.
Embodiment 3
The first solution 30g embodiment 1 prepared adds in the 2nd solution prepared by 40g embodiment 2, and after high-speed stirring 30 seconds, mixing solutions starts to turn white, CO2Gas starts to release, shifting goes to stir, proceed in mould, standing mould makes its free foaming, after 3min, lather volume is expanded to not reflation gradually, obtains foam intermediate, is warming up to 160 DEG C of heating 1h after foam intermediate moves into baking oven 60 DEG C of slaking 1h, being warming up to 250 DEG C of imidization 2h again, cooling and demolding obtains Polyamide-imide foam.
The Polyamide-imide foam embodiment of the present invention prepared carries out performance test, and detailed process is as follows:
The present invention adopts dynamic thermomechanical analysis apparatus, in a compressed mode, is measured by the second-order transition temperature of the Polyamide-imide foam obtained with the temperature rise rate of 5 �� of C/min;
The Polyamide-imide foam square-cut block that the present invention will obtain, measures its volume and quality thus calculates its apparent density;
The present invention adopts thermal weight loss TGA analysis tester, at N2Under condition, with the temperature rise rate of 10 �� of C/min, the thermal weight loss situation of prepared foam is measured; The second-order transition temperature of Polyamide-imide foam, apparent density, 5% thermal weight loss temperature, compressive strength and tensile strength, result is as shown in table 1, the performance test results of the Polyamide-imide foam that table 1 prepares for the embodiment of the present invention.
Embodiment 4
30g first solution embodiment 1 prepared adds in the 2nd solution prepared by 38g embodiment 2, and after high-speed stirring 10 seconds, mixing solutions starts to turn white, CO2Gas starts to release, shifting goes to stir, proceed in mould, standing mould makes its free foaming, after 5min, lather volume is expanded to not reflation gradually, obtains foam intermediate, is warming up to 160 DEG C of heating 1h after foam intermediate moves into baking oven 60 DEG C of slaking 1h, being warming up to 250 DEG C of imidization 2h again, cooling and demolding obtains Polyamide-imide foam.
The Polyamide-imide foam that the present invention adopts the method for the test described in the embodiment of the present invention 3 embodiment 4 to be prepared carries out performance test, obtain the second-order transition temperature of Polyamide-imide foam, apparent density, 5% thermal weight loss temperature, compressive strength and tensile strength, result is as shown in table 1, the performance test results of the Polyamide-imide foam that table 1 prepares for the embodiment of the present invention.
Embodiment 5
30g first solution embodiment 1 prepared adds in the 2nd solution prepared by 42g embodiment 2, and after high-speed stirring 20 seconds, mixing solutions starts to turn white, CO2Gas starts to release, shifting goes to stir, proceed in mould, standing mould makes its free foaming, after 2min, lather volume is expanded to not reflation gradually, obtains foam intermediate, is warming up to 160 DEG C of heating 1h after foam intermediate moves into baking oven 60 DEG C of slaking 1h, being warming up to 250 DEG C of imidization 2h again, cooling and demolding obtains Polyamide-imide foam.
The Polyamide-imide foam that the present invention adopts the technical scheme of the test described in embodiment 3 embodiment 5 to be prepared carries out performance test, obtain the second-order transition temperature of Polyamide-imide foam, apparent density, 5% thermal weight loss temperature, compressive strength and tensile strength, result is as shown in table 1, the performance test results of the Polyamide-imide foam that table 1 prepares for the embodiment of the present invention.
The performance test results of the Polyamide-imide foam that table 1 embodiment of the present invention prepares
As shown in Table 1, the density of the Polyamide-imide foam that the embodiment of the present invention prepares is low and Heat stability is good.
The above is only the preferred embodiment of the present invention; it is noted that for those skilled in the art, under the premise without departing from the principles of the invention; can also making some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (8)
1. the preparation method of a Polyamide-imide foam, it is characterised in that, comprising:
A) trimellitic acid 1,2-anhydride, whipping agent, catalyzer and tensio-active agent are mixed in a solvent, obtain the first solution;
In described steps A, solvent is selected from N-Methyl pyrrolidone, DMAC N,N' dimethyl acetamide, N, the one in dinethylformamide;
In described steps A, whipping agent is selected from methyl alcohol, ethanol, propyl alcohol, butanols, ethylene glycol, acetone, tetrahydrofuran (THF) and ethylene glycol monomethyl ether one or more and water;
One or more in described steps A, catalyzer is selected from trolamine, triethylene diamine, two (2-dimethylaminoethyl) ether, Dabco33-LV, DabcoCS90 and Polycat41 one or more and stannous octoate, dibutyl tin laurate, mercaptan dioctyl tin and dibutyltin diacetate;
In described steps A, tensio-active agent is selected from low molecular poly, one or more in DC5598, DC193, DC195, DC197, DC198, AK168, L620 and L6900;
B) the first solution and polyisocyanate solution mixed, stir, foam, obtain foam intermediate; Described whipping temp is 25 DEG C��30 DEG C;
In described polyisocyanate solution, polyisocyanates is polyphenyl polymethylene polyisocyanates;
In described polyisocyanate solution, solvent is selected from N-Methyl pyrrolidone, DMAC N,N' dimethyl acetamide, N, the one in dinethylformamide;
C) foam intermediate imidization is obtained Polyamide-imide foam.
2. preparation method according to claim 1, it is characterized in that, in described first solution, the mass ratio of trimellitic acid 1,2-anhydride, solvent, whipping agent, catalyzer and tensio-active agent is (100): (100��300): (5��28): (0.02��10): (5��40).
3. preparation method according to claim 2, it is characterised in that, in described polyisocyanate solution, the mass ratio of polyisocyanates and solvent is 1:(1��3).
4. preparation method according to claim 3, it is characterised in that, in described step B, the mass ratio of the first solution and polyisocyanate solution is 1:(0.1��2).
5. preparation method according to claim 1, it is characterised in that, in described step B, churning time is 10��30s, and described whipping temp is 25 DEG C��30 DEG C.
6. preparation method according to claim 1, it is characterised in that, in described step B, the time of foaming is 1��5min, and described blowing temperature is 25 DEG C��30 DEG C.
7. preparation method according to claim 1, it is characterised in that, in described step C, imidization temperature is 50 DEG C��300 DEG C, and the time of imidization is 3��5h.
8. a Polyamide-imide foam, it is characterised in that, prepare by the preparation method described in claim 1��7.
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| CN105295047B (en) * | 2015-11-30 | 2017-12-22 | 苏州太湖电工新材料股份有限公司 | A kind of preparation method of polyimides high polymer |
| CN109180935A (en) * | 2018-07-12 | 2019-01-11 | 溧阳华晶合成材料有限公司 | A kind of preparation method of Polyamide-imide foam |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4990543A (en) * | 1989-07-13 | 1991-02-05 | Manville Corporation | Lightweight flexible inide foam and method of producing same |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4990543A (en) * | 1989-07-13 | 1991-02-05 | Manville Corporation | Lightweight flexible inide foam and method of producing same |
Non-Patent Citations (2)
| Title |
|---|
| 水发泡剂对聚酰亚胺泡沫结构与性能的影响;詹茂盛等;《航空材料学报》;20100630;第30卷(第3期);第55-60页 * |
| 聚酰胺酰亚胺的研发新进展;吴国光;《信息记录材料》;20111231;第12卷(第3期);第12-17页 * |
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