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US 5,210,174 AGranted
Preparation process of polyimide
AssigneeMitsui Toatsu Chemicals, Inc.
InventorsShoji Tamai, Hideaki Oikawa, Masahiro Ohta, Akihiro Yamaguchi
Life of this patent
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Abstract
In a process for the preparation of polyimide by reacting a diamine compound with tetracarboxylic dianhydride in a phenol based solvent, an improved process for reacting the diamine compound with tetracarboxylic dianhydride in a solution by forming separate solutions of the tetracarboxylic dianhydride and the diamine compound and mixing the solutions and/or by dissolving tetracarboxylic dianhydride in the phenol-based solvent containing an organic base.
Claims13
A process for preparing a polyimide by reacting a diamine compound represented by the formula (I):
- H.sub.2 N--R.sub.1 --NH.sub.2 (I)
- wherein R.sub.1 is a divalent radical selected from the group consisting of an aliphatic group, alicyclic group, monocyclic aromatic group, fused polycyclic aromatic radical group and polycyclic aromatic group connected to each other through a direct bond or a bridge member, with a tetracarboxylic dianhydride having the formula (II):
- ##STR7## wherein R.sub.2 is a tetravalent radical selected from the group consisting of an aliphatic group, alicyclic group, monocyclic aromatic group, fused polycyclic aromatic group and polycyclic aromatic group connected to each other through a direct bond or a bridge member, to prepare a polyimide having a recurring units represented by the formula (III):
- ##STR8## wherein R.sub.1 and R.sub.2 are individually selected from the group consisting of an aliphatic group, alicyclic group, monocyclic aromatic group, fused polycyclic aromatic group and polycyclic aromatic group connected to each other through a direct bond or a bridge member, R.sub.1 is a divalent radical and R.sub.2 is a tetravalent radical;
- comprising the steps of dissolving the diamine compound of the formula (I) and the tetracarboxylic dianhydride of the formula (II) in separate phenol-based solvents selected from the group consisting of phenol, m-cresol, o-cresol, p-cresol, cresylic acid, ethylphenol, isopropylphenol, tert-butylphenol, xylenol, chlorophenol, dichlorophenol, phenylphenol and mixtures thereof, respectively, mixing the resultant monomer solutions and reacting at a temperature of from 100.degree. to 300.degree. C. to prepare the corresponding polyimide.
2 more elements
A process for preparing a polyimide by reacting a diamine compound represented by the formula (I):
- H.sub.2 N--R.sub.1 --NH.sub.2 (I)
- wherein R.sub.1 is a divalent radical selected from the group consisting of an aliphatic group, alicyclic group, monocyclic aromatic group, fused polycyclic aromatic radical group and polycyclic aromatic group connected to each other through a direct bond or a bridge member, with a tetracarboxylic dianhydride having the formula (II):
- ##STR11## wherein R.sub.2 is a tetravalent radical selected from the group consisting of an aliphatic group, alicyclic group, monocyclic aromatic group, fused polycyclic aromatic group and polycyclic aromatic group connected to each other through a direct bond or a bridge member, to prepare a polyimide having a recurring unit represented by the formula (III):
- ##STR12## wherein R.sub.1 and R.sub.2 are individually selected from the group consisting of an aliphatic group, alicyclic group, monocyclic aromatic group, fused polycyclic aromatic group and polycyclic aromatic group connected to each other through a direct bond or a bridge member, R.sub.1 is a divalent radical and R.sub.2 is a tetravalent radical;
- comprising the steps of reacting the diamine compound of the formula (I) and the tetracarboxylic dianhydride of the formula (II) in the presence of an organic base selected from the group consisting of triethylamine, tributylamine, tripentylamine, N,N-dimethylaniline, N,N-diethylaniline, pyridine, .alpha.-picoline, .beta.-picoline, .gamma.-picoline, 2,4-lutidine, 2,6-lutidine, quinoline and isoquinoline in a phenol based solvent selected from the group consisting of phenol, m-cresol, o-cresol, p-cresol, cresylic acid, ethylphenol, isopropylphenol, tert-butylphenol, xylenol, chlorophenol, dichlorophenol, phenylphenol and mixtures thereof to obtain a solution of a polyamic acid represented by the formula (IV):
- ##STR13## wherein R.sub.1 and R.sub.2 are individually selected from the group consisting of an aliphatic alicyclic, monoaromatic, and condensed aromatic radical and noncondensed aromatic radical connected to each other through a direct bond or a bridge member, R.sub.1 is a divalent radical and R.sub.2 is a tetravalent radical, and heating the solution to a temperature of from 100.degree. to 300.degree. C. to prepare corresponding polyimide.
3 more elements
Dependencies are inferred from the claim text.