CN103214688A - Polyamide-imide foam and preparation method thereof - Google Patents
Polyamide-imide foam and preparation method thereof Download PDFInfo
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- CN103214688A CN103214688A CN2013101726637A CN201310172663A CN103214688A CN 103214688 A CN103214688 A CN 103214688A CN 2013101726637 A CN2013101726637 A CN 2013101726637A CN 201310172663 A CN201310172663 A CN 201310172663A CN 103214688 A CN103214688 A CN 103214688A
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Abstract
The invention provides a preparation method of polyamide-imide foam. The preparation method comprises the steps of: mixing trimellitil anhydride, a foaming agent, a catalyst and a surface active agent in a solvent to obtain a first solution; mixing the first solution with polyisocyanate, stirring and foaming to obtain a foam intermediate; and imidizing the foam intermediate to obtain the polyamide-imide foam. The trimellitil anhydride and polyisocyanate are adopted for polymerization reaction, and simultaneously, the gas is generated to foam and shape a polymer. The polyamide-imide foam obtained by adopting the trimellitil anhydride and polyisocyanate for polymerization reaction is high in thermal stability and low in density; and according to the polyamide-imide foam and the preparation method thereof, no complicated preparation conditions of high temperature for reaction are needed, and the technology is simple.
Description
Technical field
The present invention relates to technical field of polymer materials, especially relate to a kind of polyamidoimide foam and preparation method thereof.
Background technology
Polyamidoimide is a base polymer that contains the amide group of heat-stable imide ring and flexibility in the class backbone structure simultaneously.Polyamidoimide has the feature performance benefit of polymeric amide and polyimide concurrently, has good thermotolerance, dielectricity, mechanical property and chemical stability.Though the amide group thermotolerance that contains in the main chain of polyamidoimide decreases than polyimide, amide group can make the molecule chain rigidity reduce, and solubility is improved, thereby improves the rheological property and the processing characteristics of polymkeric substance.Simultaneously, polyamidoimide has the electro permanent magnetic under excellent anti-ablation property and high temperature, the high frequency condition, therefore can make ablator, magnetic-permeable material and the structured material of aircraft.Polyamidoimide has good adhesiveproperties to metal, 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 structural parts such as various gears, roller, bearing through mold pressing.
Except that above purposes, a kind of important use of polyamidoimide is to be processed into foam materials, compared to conventional foam such as urethane, polyethylene, polystyrene, the polyamidoimide foam has excellent flame, and difficult combustion, low cigarette, no obnoxious flavour release, radiation hardness, resistance to chemical attack also can be used under hot conditions.Prior art discloses multiple polyamidoimide foamy preparation method, after the hexanolactam reaction of U.S. Pat 4604409 with the dianhydride of fragrance and fat, add isocyanate reaction, obtain the polyamide-imide foam materials that main chain contains six carbocyclic aliphatic chains.But introduced a large amount of fat chain structures in this polymer chain, the poor heat stability of the foam materials of acquisition.
U.S. Pat 4990543 discloses a kind of polyamidoimide foamy preparation method: vulcabond and trimellitic acid 1,2-anhydride, the polymerization of ketone acid anhydride obtain oligopolymer, under the condition of strictness control carbon dioxide releasing amount, and the precursor powder of preparation foaming.Then 230 ° of C foaming.But this technology precursor powder complicated process of preparation, the blowing temperature height.
U.S. Pat 4960549 discloses utilizes extrusion equipment to prepare polyamide-imide foamy method.But the comparatively complicated and foam densities that makes of this foam process equipment is up to 300g/cm
3, can't obtain more low-density soft foam materials.
Summary of the invention
In view of this, the technical problem to be solved in the present invention is to provide a kind of polyamidoimide foam, and polyamidoimide foamy technology provided by the invention is simple, density is low and the thermostability height.
The invention provides a kind of polyamidoimide foamy preparation method, comprising:
A) trimellitic acid 1,2-anhydride, whipping agent, catalyzer and tensio-active agent are mixed in solvent, obtain first solution;
B) first solution and polyisocyanate solution are mixed, stir, foam, obtain foam intermediate;
C) the foam intermediate imidization is obtained the polyamidoimide foam.
Preferably, solvent is selected from N-Methyl pyrrolidone in the described steps A, N, N '-N,N-DIMETHYLACETAMIDE, N, a kind of in N '-dimethyl formamide;
Whipping agent is selected from one or more in water, methyl alcohol, ethanol, propyl alcohol, butanols, ethylene glycol, acetone, tetrahydrofuran (THF) and the ethylene glycol monomethyl ether in the described steps A;
Catalyzer is selected from one or more in trolamine, triethylene diamine, triethylenediamine, two (2-dimethylaminoethyl) ether, Dabco33-LV, Dabco CS90, Polycat41, stannous octoate, dibutyl tin laurate, mercaptan dioctyl tin and the dibutyltin diacetate in the described steps A;
Tensio-active agent is selected from low molecular poly in the described steps A, one or more among DC5598, DC193, DC195, DC197, DC198, KH550, AK168, L620 and the L6900.
Preferably, the mass ratio of trimellitic acid 1,2-anhydride, solvent, whipping agent, catalyzer and tensio-active agent is (100) in described first solution: (100～300): (5～28): (0.02～10): (5～40).
Preferably, the mass ratio of polyisocyanates and solvent is 1:(1～3 in the described polyisocyanate solution).
Preferably, the mass ratio of first solution and polyisocyanate solution is 1:(0.1～2 among the described step B).
Preferably, polyisocyanates is selected from polyphenyl polymethylene polyisocyanates, toluene two different hydrogen acid ethers, diphenylmethanediisocyanate, isophorone diisocyanate, xylylene diisocyanate and the tetramethylxylylene diisocyanate one or more in the described polyisocyanate solution;
Solvent is selected from N-Methyl pyrrolidone in the described polyisocyanate solution, N, N '-N,N-DIMETHYLACETAMIDE, N, a kind of in N '-dimethyl formamide.
Preferably, churning time is 10～30s among the described step B, and described whipping temp is 25 ℃～30 ℃.
Preferably, the time of foaming among the described step B is 1～5min, and described blowing temperature is 25 ℃～30 ℃.
Preferably, imidization tool temperature is 50 ℃～300 ℃ among the described step C, and the time of imidization is 3～5h.
The present invention also provides a kind of polyamidoimide foam, and described preparation method prepares by technique scheme.
Compared with prior art, a kind of polyamidoimide foamy preparation method comprises: trimellitic acid 1,2-anhydride, whipping agent, catalyzer and tensio-active agent are mixed in solvent, obtain first solution; First solution and polyisocyanate solution are mixed, stir, foam, obtain foam intermediate; The foam intermediate imidization is obtained the polyamidoimide foam.The present invention adopts trimellitic acid 1,2-anhydride and polyisocyanates polymerization reaction take place, produces gas simultaneously and makes polymer foaming finalize the design.The present invention adopts trimellitic acid 1,2-anhydride and polyisocyanates polyreaction, and the polyamidoimide foam thermal stability height and the density that obtain are low; The present invention's reaction need not complicated preparation conditions such as high temperature, and technology is simple.Experimental result shows that the polyamidoimide foamy apparent density that the present invention prepares is 10.9Kg/m
3, glass transition temp is 280 ℃, and 5% thermal weight loss temperature is 326 ℃, and compressive strength is 0.07144MPa, and tensile strength is 0.1078MPa.
Embodiment
A kind of polyamidoimide foamy preparation method comprises:
A) trimellitic acid 1,2-anhydride, whipping agent, catalyzer and tensio-active agent are mixed in solvent, obtain first solution;
B) first solution and polyisocyanate solution are mixed, stir, foam, obtain foam intermediate;
C) the foam intermediate imidization is obtained the polyamidoimide foam.
The present invention at first mixes trimellitic acid 1,2-anhydride, whipping agent, catalyzer and tensio-active agent in solvent, obtain first solution.The present invention is for described hybrid mode and unrestricted, and hybrid mode well known to those skilled in the art gets final product, and is preferably to mix, and the described temperature that mixes is preferably 25 ℃～30 ℃.
In the present invention, solvent is preferably selected from N-Methyl pyrrolidone in the described steps A, N, N '-N,N-DIMETHYLACETAMIDE, N, a kind of in N '-dimethyl formamide; More preferably be selected from N, N '-N,N-DIMETHYLACETAMIDE and N, a kind of in N '-dimethyl formamide.
In the present invention, whipping agent is preferably selected from water, methyl alcohol, ethanol, propyl alcohol, butanols, ethylene glycol, acetone, tetrahydrofuran (THF) and the ethylene glycol monomethyl ether one or more in the described steps A; More preferably be selected from water, methyl alcohol, ethanol, propyl alcohol, butanols, ethylene glycol, the acetone one or more; Most preferably be selected from water, methyl alcohol, ethanol, the propyl alcohol one or more.
In the present invention, catalyzer is preferably selected from trolamine, triethylene diamine, triethylenediamine, two (2-dimethylaminoethyl) ether, Dabco33-LV, Dabco CS90, Polycat41, stannous octoate, dibutyl tin laurate, mercaptan dioctyl tin and the dibutyltin diacetate one or more in the described steps A; More preferably be selected from trolamine, triethylene diamine, stannous octoate, dibutyl tin laurate, mercaptan dioctyl tin and the dibutyltin diacetate one or more; Most preferably be selected from trolamine, stannous octoate, dibutyl tin laurate and the dibutyltin diacetate one or more.
In the present invention, tensio-active agent is preferably selected from low molecular poly in the described steps A, one or more among DC5598, DC193, DC195, DC197, DC198, KH550, AK168, L620 and the L6900; More preferably be selected from polyoxyethylene glycol, one or more among DC5598, DC193, DC195, DC197, DC198 and the L620; Most preferably be selected from polyoxyethylene glycol, one or more among DC193, DC195, the DC197.
In the present invention, the mass ratio of trimellitic acid 1,2-anhydride, solvent, whipping agent, catalyzer and tensio-active agent is preferably (100) in described first solution: (100～300): (5～28): (0.02～10): (5～40); The mass ratio of trimellitic acid 1,2-anhydride, solvent, whipping agent, catalyzer and tensio-active agent more preferably (100) in the described steps A: (120～280): (8～25): (0.1～8): (8～35).
After obtaining first solution, first solution and polyisocyanate solution are mixed, stir, foam, obtain foam intermediate.Be specially in first solution adding polyisocyanate solution, mix, pour in the mould, free foaming obtains foam intermediate.Described churning time is preferably 10～30 seconds, and described whipping temp is preferably 25 ℃～30 ℃.Stir back solution and begin to turn white CO
2Gas begins to emit.The time of described foaming is preferably 1～5min, more preferably 3～5min.Described blowing temperature is preferably 25 ℃～30 ℃.
The mass ratio of trimellitic acid 1,2-anhydride, solvent, whipping agent, catalyzer and tensio-active agent is preferably (100) in described first solution: (100～300): (5～28): (0.02～10): (5～40); The mass ratio of trimellitic acid 1,2-anhydride, solvent, whipping agent, catalyzer and tensio-active agent more preferably (100) in the described steps A: (120～280): (8～25): (0.1～8): (8～35).The mass ratio of polyisocyanates and solvent is preferably 1:(1～3 in the described polyisocyanate solution).The mass ratio of above-mentioned first solution and polyisocyanate solution is preferably 1:(0.1～2).
In the present invention, polyisocyanates is preferably selected from polyphenyl polymethylene polyisocyanates, toluene two different hydrogen acid ethers, diphenylmethanediisocyanate, isophorone diisocyanate, xylylene diisocyanate and the tetramethylxylylene diisocyanate one or more in the described polyisocyanate solution; More preferably be selected from polyphenyl polymethylene polyisocyanates, toluene two different hydrogen acid ethers, diphenylmethanediisocyanate and the isophorone diisocyanate one or more; Most preferably be selected from polyphenyl polymethylene polyisocyanates, diphenylmethanediisocyanate and the isophorone diisocyanate one or more.
Solvent is preferably selected from N-Methyl pyrrolidone in the described polyisocyanate solution, N, and N '-N,N-DIMETHYLACETAMIDE, N, a kind of in N '-dimethyl formamide more preferably is selected from N, N '-N,N-DIMETHYLACETAMIDE and N, a kind of in N '-dimethyl formamide.
In the present invention, solvent can be identical in solvent and the polyisocyanate solution in described first solution, also can be different, the present invention to this and unrestricted.
After obtaining foam intermediate, the foam intermediate imidization is obtained the polyamidoimide foam.Described imidization imidization temperature is preferably 50 ℃～300 ℃, and the time of imidization is preferably 3～5h.Described imidization is preferably slaking, desolventizes and the imidization three phases, is specially slaking 40min～80min under 50 ℃～100 ℃ temperature; Under 100 ℃～200 ℃ temperature, desolventize 40min～90min; At 200 ℃～300 ℃ imidization 1.5h～2.5h.Preferred imidization postcooling obtains the polyamidoimide foam.The present invention is for the described type of cooling and unrestricted, and the type of cooling well known to those skilled in the art gets final product.
The present invention adopts trimellitic acid 1,2-anhydride and polyisocyanates polymerization reaction take place, produces gas simultaneously and makes polymer foaming finalize the design.The present invention adopts trimellitic acid 1,2-anhydride and polyisocyanates polyreaction, and the polyamidoimide foam thermal stability height and the density that obtain are low; The present invention's reaction need not complicated preparation conditions such as high temperature, and technology is simple.
The polyamidoimide foam that the present invention preferably prepares 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, under compact model, with the temperature rise rate of 5 ° of C/min the polyamidoimide foamy second-order transition temperature that obtains is measured;
The present invention is the polyamidoimide foam square-cut piece that obtains, thereby measures its volume and quality calculates its apparent density;
The present invention adopts thermal weight loss TGA analysis tester, at N
2Under the condition, prepared foamy thermal weight loss situation is measured with the temperature rise rate of 10 ° of C/min; Polyamidoimide foamy second-order transition temperature, apparent density, 5% thermal weight loss temperature,
In order to further specify the present invention, polyamidoimide foam provided by the invention and preparation method thereof is described in detail below in conjunction with embodiment.
Embodiment 1
148g trimellitic acid 1,2-anhydride, 10g methyl alcohol, 12g deionized water, 17g DC-193,6.5g polyoxyethylene glycol, 0.1g trolamine and 0.1g dibutyl tin laurate are joined 120g N respectively, in N '-dimethyl formamide (DMF) solution, the stirring at room dissolving evenly obtains first solution.
Embodiment 2
The 100g polyphenyl polymethylene polyisocyanates is dissolved in 100g N, in N '-dimethyl formamide, obtains second solution.
Embodiment 3
The first solution 30g that embodiment 1 is prepared adds in second solution of 40g embodiment 2 preparations, and mixing solutions begins to turn white CO after the high-speed stirring 30 seconds
2Gas begins to emit, remove stirring, change in the mould, leave standstill mould and make its free foaming, lather volume is expanded to gradually no longer and expands behind the 3min, obtains foam intermediate, is warming up to 160 ℃ of heating 1h after foam intermediate is moved into 60 ℃ of slaking 1h of baking oven, be warming up to 250 ℃ of imidization 2h again, cooling and demolding obtains the polyamidoimide foam.
The polyamidoimide foam that the embodiment of the invention is prepared carries out performance test, and detailed process is as follows:
The present invention adopts dynamic thermomechanical analysis apparatus, under compact model, with the temperature rise rate of 5 ° of C/min the polyamidoimide foamy second-order transition temperature that obtains is measured;
The present invention is the polyamidoimide foam square-cut piece that obtains, thereby measures its volume and quality calculates its apparent density;
The present invention adopts thermal weight loss TGA analysis tester, at N
2Under the condition, prepared foamy thermal weight loss situation is measured with the temperature rise rate of 10 ° of C/min; Polyamidoimide foamy second-order transition temperature, apparent density, 5% thermal weight loss temperature, compressive strength and tensile strength, the result is as shown in table 1, the polyamidoimide foamy The performance test results that table 1 prepares for the embodiment of the invention.
Embodiment 4
30g first solution that embodiment 1 is prepared adds in second solution of 38g embodiment 2 preparations, and mixing solutions begins to turn white CO after the high-speed stirring 10 seconds
2Gas begins to emit, remove stirring, change in the mould, leave standstill mould and make its free foaming, lather volume is expanded to gradually no longer and expands behind the 5min, obtains foam intermediate, is warming up to 160 ℃ of heating 1h after foam intermediate is moved into 60 ℃ of slaking 1h of baking oven, be warming up to 250 ℃ of imidization 2h again, cooling and demolding obtains the polyamidoimide foam.
The present invention adopts the method for the embodiment of the invention 3 described tests that the polyamidoimide foam that embodiment 4 prepares is carried out performance test, obtain polyamidoimide foamy second-order transition temperature, apparent density, 5% thermal weight loss temperature, compressive strength and tensile strength, the result is as shown in table 1, the polyamidoimide foamy The performance test results that table 1 prepares for the embodiment of the invention.
Embodiment 5
30g first solution that embodiment 1 is prepared adds in second solution of 42g embodiment 2 preparations, and mixing solutions begins to turn white CO after the high-speed stirring 20 seconds
2Gas begins to emit, remove stirring, change in the mould, leave standstill mould and make its free foaming, lather volume is expanded to gradually no longer and expands behind the 2min, obtains foam intermediate, is warming up to 160 ℃ of heating 1h after foam intermediate is moved into 60 ℃ of slaking 1h of baking oven, be warming up to 250 ℃ of imidization 2h again, cooling and demolding obtains the polyamidoimide foam.
The present invention adopts the technical scheme of embodiment 3 described tests that the polyamidoimide foam that embodiment 5 prepares is carried out performance test, obtain polyamidoimide foamy second-order transition temperature, apparent density, 5% thermal weight loss temperature, compressive strength and tensile strength, the result is as shown in table 1, the polyamidoimide foamy The performance test results that table 1 prepares for the embodiment of the invention.
The polyamidoimide foamy The performance test results that table 1 embodiment of the invention prepares
As shown in Table 1, the low and Heat stability is good of polyamidoimide foamy density for preparing of the embodiment of the invention.
The above only is a preferred implementation of the present invention; should be pointed out that for those skilled in the art, under the prerequisite that does not break away from the principle of the invention; can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (10)
1. a polyamidoimide foamy preparation method is characterized in that, comprising:
A) trimellitic acid 1,2-anhydride, whipping agent, catalyzer and tensio-active agent are mixed in solvent, obtain first solution;
B) first solution and polyisocyanate solution are mixed, stir, foam, obtain foam intermediate;
C) the foam intermediate imidization is obtained the polyamidoimide foam.
2. preparation method according to claim 1 is characterized in that solvent is selected from N-Methyl pyrrolidone in the described steps A, N, N '-N,N-DIMETHYLACETAMIDE, N, a kind of in N '-dimethyl formamide;
Whipping agent is selected from one or more in water, methyl alcohol, ethanol, propyl alcohol, butanols, ethylene glycol, acetone, tetrahydrofuran (THF) and the ethylene glycol monomethyl ether in the described steps A;
Catalyzer is selected from one or more in trolamine, triethylene diamine, triethylenediamine, two (2-dimethylaminoethyl) ether, Dabco33-LV, Dabco CS90, Polycat41, stannous octoate, dibutyl tin laurate, mercaptan dioctyl tin and the dibutyltin diacetate in the described steps A;
Tensio-active agent is selected from low molecular poly in the described steps A, one or more among DC5598, DC193, DC195, DC197, DC198, KH550, AK168, L620 and the L6900.
3. preparation method according to claim 1, it is characterized in that the mass ratio of trimellitic acid 1,2-anhydride, solvent, whipping agent, catalyzer and tensio-active agent is (100) in described first solution: (100～300): (5～28): (0.02～10): (5～40).
4. preparation method according to claim 3 is characterized in that, the mass ratio of polyisocyanates and solvent is 1:(1～3 in the described polyisocyanate solution).
5. preparation method according to claim 4 is characterized in that, the mass ratio of first solution and polyisocyanate solution is 1:(0.1～2 among the described step B).
6. preparation method according to claim 1, it is characterized in that polyisocyanates is selected from one or more in polyphenyl polymethylene polyisocyanates, toluene two different hydrogen acid ethers, diphenylmethanediisocyanate, isophorone diisocyanate, xylylene diisocyanate and the tetramethylxylylene diisocyanate in the described polyisocyanate solution;
Solvent is selected from N-Methyl pyrrolidone in the described polyisocyanate solution, N, N '-N,N-DIMETHYLACETAMIDE, N, a kind of in N '-dimethyl formamide.
7. preparation method according to claim 1 is characterized in that, churning time is 10～30s among the described step B, and described whipping temp is 25 ℃～30 ℃.
8. preparation method according to claim 1 is characterized in that, the time of foaming among the described step B is 1～5min, and described blowing temperature is 25 ℃～30 ℃.
9. preparation method according to claim 1 is characterized in that, imidization tool temperature is 50 ℃～300 ℃ among the described step C, and the time of imidization is 3～5h.
10. a polyamidoimide foam is characterized in that, described preparation method prepares by claim 1～9.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105295047A (en) * | 2015-11-30 | 2016-02-03 | 苏州太湖电工新材料股份有限公司 | Polyimide polymer preparation method |
| 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 |
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|---|---|---|---|---|
| US4990543A (en) * | 1989-07-13 | 1991-02-05 | Manville Corporation | Lightweight flexible inide foam and method of producing same |
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2013
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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 |
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| 吴国光: "聚酰胺酰亚胺的研发新进展", 《信息记录材料》, vol. 12, no. 3, 31 December 2011 (2011-12-31), pages 12 - 17 * |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105295047A (en) * | 2015-11-30 | 2016-02-03 | 苏州太湖电工新材料股份有限公司 | Polyimide polymer preparation method |
| 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 |
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