Process for producing synthetic resin film having molecular orientation controlled in md direction
A technology of synthetic resin and manufacturing method, which is applied in the fields of printed circuit manufacturing, flat products, and other household appliances, etc., and can solve problems such as film wrinkling, wrinkling, and difficulty in stably maintaining the balance of MD/TD characteristics
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[0104] Hereafter, although an Example demonstrates this invention concretely, this invention is not limited only to an Example. In addition, evaluation of the molecular orientation angles of the thin films in Examples and Comparative Examples was performed as described below. In addition, Table 1 summarizes the production conditions of the thin films of Examples and Comparative Examples.
[0105] (Molecular orientation angle of film)
[0106] A sample of 4 cm x 4 cm was cut out and measured using a microwave molecular orientation meter MOA2012A manufactured by Oji Instruments.
[0107] Here, the molecular orientation angle θ is defined as follows.
[0108] Using the MOA2012 model, the orientation direction of molecules in the film plane (the maximum orientation of ε', where ε' is the dielectric constant of the sample) can be known as an angle value. In the present invention, a straight line indicating the orientation direction is taken as the "orientation axis" of the sampl...
manufacture example 1
[0114] Polymerize pyromellitic dianhydride / 4,4'-diphenylamine oxide / p-phenylenediamine in a molar ratio of 1 / 0.75 / 0.25 in N,N'-dimethylacetamide solvent, Make the solids fraction 18%. Specifically, 4,4'-diphenylamine oxide, which is 75 mol% relative to the total diamine components, is dissolved in N,N'-dimethylacetamide solvent, and then the full amount of pyromellitic dianhydride (ie relative An acid-terminated prepolymer was prepared from the charged diamine component of 133% acid anhydride). Then add the rest of the diamine component (ie, p-phenylenediamine) to the acid-terminated prepolymer solution, and add the insufficient amount of diamine so that it reacts substantially equimolarly with the total acid component to obtain a polymerization solution.
[0115]After cooling the polymerization solution to about 0°C, 2.0 moles of acetic anhydride and 0.5 moles of isoquinoline were added to 1 mole of amic acid in the polyamic acid organic solvent solution cooled to about 0°C,...
manufacture example 2
[0117] Put pyromellitic dianhydride / terephthalic acid anhydride / 4,4'-diaminodiphenyl ether / p-phenylenediamine in molar ratio of 0.50 / 0.50 / 0.50 / 0.50 Ratio, the polymerization was carried out under N, N'-dimethylacetamide solvent, so that the solid content was 18%. Specifically, 50 mol% of 4,4'-diaminodiphenyl ether and 50 mol% of p-phenylenediamine relative to all diamine components were dissolved in N,N'-diamine Then, 50 mol% of terephthalic acid dianhydride (trimellitic acid monoester anhydride) was added to the methyl acetamide solvent to obtain an amine-terminated prepolymer. Then, add remaining acid dianhydride components (i.e., pyromellitic dianhydride) to this amine-terminated prepolymer solution, add insufficient acid dianhydride components, so that it becomes substantially equimolar with all acid components, and react A polymerization solution was prepared.
[0118] After cooling the polymerization solution to about 0°C, add 2.1 moles of acetic anhydride and 1.1 mole...
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