Resin precursor, resin composition containing said resin precursor, resin film, method for producing said resin film, laminate, and method for producing said laminate
A precursor and resin technology, applied in chemical instruments and methods, synthetic resin layered products, coatings, etc., can solve problems such as low transmittance and difficult to use in fields requiring transparency
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Embodiment 1
[0268] In a 3L detachable flask equipped with a stirring bar equipped with an oil bath, introduce nitrogen gas, add 1000g of NMP, and add 232.4g of 3,3-(diaminodiphenyl)sulfone (defined as diaminodiphenyl)sulfone while stirring. Amine 1), followed by adding 218.12 g of pyromellitic dianhydride (specified as tetracarboxylic anhydride 1), and stirring at room temperature for 30 minutes. It was heated up to 50° C., and after stirring for 12 hours, 105.6 g of both-terminal amine-modified methylphenyl silicone oil (manufactured by Shin-Etsu Chemical Co., Ltd.: X22-1660B-3 (number average molecular weight 4400)) ( It is defined as a silicon group-containing diamine) was dissolved in 298 g of NMP, and was added dropwise using a dropping funnel. After heating up to 80 degreeC and stirring for 1 hour, the oil bath was removed, it returned to room temperature, and the NMP solution (henceforth, also referred to as a varnish) of a transparent polyamic acid was obtained. Table 1 shows the...
Embodiment 2～33、49～58
[0270] In the same manner as in Example 1, the types of diamine 1, tetracarboxylic anhydride 1, and silicon group-containing diamine, and their added masses were changed to those described in Table 1, respectively, and the same operation as in Example 1 was performed to obtain a varnish. In addition, the addition amount of NMP shown in Table 1 and Table 2 represents the total amount of NMP contained in the final varnish, and is the mass containing 298 g of NMP for diluting the silicon group containing diamine. The composition and the weight average molecular weight (Mw) of the obtained polyamic acid are shown in Table 1, Table 2, and Table 7, respectively. In addition, the test results of the films cured at 350°C are shown in Table 4, Table 5, and Table 8, respectively. The official compound names of the abbreviated compound names described in Tables 1 to 6 are described below.
[0271] 3,3-DAS: 3,3-(Diaminodiphenyl)sulfone
[0272] 4,4-DAS: 4,4-(Diaminodiphenyl)sulfone
[...
Embodiment 34
[0290] Into a 3L detachable flask equipped with a stirring bar equipped with an oil bath, introduce nitrogen gas, add 1274g of NMP, and add 4,4'-oxodiphthalic dianhydride (hereinafter referred to as ODPA) (regulated as Tetracarboxylic anhydride 1), while stirring, 105.6 g of both-terminal amine-modified methyl phenyl silicone oil (manufactured by Shin-Etsu Chemical Co., Ltd.: X22-1660B-3 (number average molecular weight 4400)) (specified as containing A solution obtained by dissolving silicon-based diamine) in 298 g of NMP was added dropwise using a dropping funnel. After stirring at room temperature for 1 hour, 149.9 g of 2,2'-bis(trifluoromethyl)benzidine (hereinafter referred to as TFMB) (defined as diamine 2) was added while stirring, and then 116.2 g of g of 3,3-DAS and stirred at room temperature for 1 hr. Next, it heated up at 50 degreeC, added 147.1g of BPDA (prescribed as tetracarboxylic anhydride 2), and stirred for 12 hours. After heating up this to 80 degreeC and...
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