专利摘要:
A method for producing polyimbdases by reacting hexamethylenediamine or diaminodiphenshchmetane, or 4,4-diaminodiphenyl ester and tetracarboxylic acid dianhydride when heated to 160-183 ° C in an organic solvent, characterized in that, in order to increase the heat resistance and solubility of the product, it will be the same. 2,2,3,3-tetracarboxydiphenyl ether is used.
公开号:SU1136748A3
申请号:SU742033203
申请日:1974-06-14
公开日:1985-01-23
发明作者:Такекоси Тару
申请人:Дженерал Электрик Компани (Фирма);
IPC主号:
专利说明:

WITH/)
WITH
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N |
00 The invention relates to the production of polyimides. The closest to the invention to the technical essence is the method of producing polyimide B by the reaction of hexamethylenediamine, diaminodiphenylmethane or 4,4-diaminodiphenyl ether and dianhydride 3,3, 4,4-tetracarboxydiphenyl ether at 160-183 ° C in an organic solvent. polyimides do not dissolve in organic solvents, and thus make them difficult to use. The purpose of the invention is to increase the heat resistance and solubility of the final product. The goal is achieved by agreeing to process for the preparation of polyimides by reaction of hexamethylene diamine or diaminodiphenylmethane, or diaminodiphenyl ether and 4,4 tetracarboxylic acid dianhydride with heating to a medium 160-183S Cesky organi solvent dianhydride as tetracarboxylic acid is 2,2, 3 3 tetrakarboksidifenilovy ether. The polyimides obtained by the proposed method are soluble in amide solvents, (V-crezole, N-methyl pyrrolidone). In addition, the proposed polyimides have a higher glass transition temperature - about. True viscosity is 0.10, 9 dl / g in m Polyimides can be used for injection molding in a mixture with fillers, for example silicon compounds, glass fibers, etc. Polyimide solutions in phenolic solvents can be used to prepare compounds for coating wires. Dian hydride 2.2 , 3,3-tetracarboxydiphenyl ether is obtained by condensation of 3-nitrophthalic anhydride in the presence of a catalytic amount of nitrite in an organic solvent or melt. Sodium nitrite is used up to 5% by weight of the condensation mixture. In the practical implementation of the method, the reaction between the diamine and dianhydride of 2,2, 3, 3-tetracarboxyphenyl ether carried out in an organic solvent medium, for example, a phenolic solvent, such as a mixture of phenols, n-, / and -cresols, ortho-dichlorobenzene; benzene, toluene, xylene, chlorobenzene, etc. are suitable. The order of administration of reagents is irrelevant. The reaction is preferably carried out in an atmosphere of inert gas, for example nitrogen. The solvent is used in an amount to ensure that the solids content of the solution is from 1 to 90%. The reaction is carried out at 160-183 ° C. The reaction mixture can be stirred to facilitate the contact of the reactants. To obtain a polymer with an optimal molecular weight, the same number of moles of reagents can be used. However, 0.5-2 mol or preferably 0.8-1.1 mol dianhydride per mol of diamine can be used. The reaction is carried out for 0.520 hours, depending on the temperature, degree of overheating, and the nature of the reagents. Water should be removed during polymer formation. The course of the reaction can be determined by the amount of water formed as a percentage of its theoretical amount. A mixture of solvents consisting of a well-boiling azeotropic solvent and a higher boiling point solvent can be used. After completion of the reaction, the polyimido ester can be isolated by draining the cooled polymer solution into a precipitant, for example methanol, followed by washing by filtration. Example 1. A mixture of 3.638 wt.h. 2,2, 3,3-tetracarboxydiphenyl ether dianhydride, 2.006 parts by weight diaminodiphenyl ether, 26 weight.h. orthodichlorobenzene, 20,06 weight.h. L-cresol and 4.3 wt.h. The toluene is heated under reflux for 3 hours, continuously removing water. A yellowish, transparent reaction mixture is obtained, which is poured into methanol to precipitate. The yield is 97.4%. True viscosity: 0.407 dl / g in dimethylformamide. The polymer can be represented by the following formula:
权利要求:
Claims (1)
[1]
METHOD FOR PRODUCING POLYIMIDES by reacting hexamethylene diamine or diaminodiphenylmethane, or 4,4'-diaminodiphenyl ether and tetracarboxylic acid dianhydride when heated to 160-183 ° C in an organic solvent, characterized in that, in order to increase the heat resistance and solubility of the final product, it is used as a dian tetracarboxylic acid use 2,2 ', 3,3'-tetracarboxydiphenyl ether.
OO O * m
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同族专利:
公开号 | 公开日
FR2300103B1|1979-02-16|
JPS58103529A|1983-06-20|
JPS5033478A|1975-03-31|
FR2300103A1|1976-09-03|
DK155013B|1989-01-23|
SE417432B|1981-03-16|
BR7405089D0|1975-01-21|
IT1015233B|1977-05-10|
DK332574A|1975-03-17|
SE7408145L|1974-12-23|
AU6775574A|1975-10-16|
GB1464009A|1977-02-09|
DD112461A5|1975-04-12|
DE2416595A1|1975-01-16|
JPS5846244B2|1983-10-15|
DE2416595C2|1984-01-12|
DK155013C|1989-05-29|
引用文献:
公开号 | 申请日 | 公开日 | 申请人 | 专利标题

US3234181A|1961-03-15|1966-02-08|Du Pont|Melt-fabricable end-capped aromatic polymides|US4098800A|1977-04-18|1978-07-04|General Electric Company|Process for preparing polyetheramide-acids|
JPS5936527U|1982-08-31|1984-03-07|
JPS5962414A|1982-10-01|1984-04-09|Toyo Seikan Kaisha Ltd|Method and device for expanding pouch mouth section|
EP0167020B1|1984-06-30|1988-11-23|Akzo Patente GmbH|Flexible polyimide multilayer laminate|
DE3448075C2|1984-08-07|1987-07-09|Simro Ag, Chur, Ch|
DE3506526A1|1985-02-25|1986-08-28|Akzo Gmbh, 5600 Wuppertal|PRINTED SWITCHING ELEMENT WITH POLYIMIDE CONTAINER|
US4835249A|1986-12-31|1989-05-30|General Electric Company|Process for preparing polyimides|
法律状态:
优先权:
申请号 | 申请日 | 专利标题
US37274173A| true| 1973-06-22|1973-06-22|
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