Thermosetting polyimide resin composition and method for producing polyimide resin
A technology of polyimide resin and manufacturing method, which is applied in printed circuit manufacturing, electrical components, printed circuit, etc., can solve the problems of hard and brittle, poor tensile elongation, high dielectric constant and dielectric loss angle, etc. Achieve good heat resistance, low dielectric constant, and low dielectric loss tangent
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Embodiment 1
[0080]In a 20-liter flask with a stirring device, a thermometer, and a condenser, add 4951 grams of diethylene glycol methyl ethyl ether acetate (hereinafter referred to as EDGA) and isophorone diisocyanate derived isocyanate Polyisocyanate with a cyanurate ring (hereinafter referred to as IPDI-N. The isocyanate group content is 18.2%, and the polyisocyanate with an isocyanurate ring is 85%) is 2760 g (12 moles of isocyanate groups), and POLYTAIL HA (Hydrogenated liquid polybutadiene with hydroxyl groups at both ends manufactured by Mitsubishi Chemical Corporation, number average molecular weight 2,100, hydroxyl value 51.2 mgKOH / g) 2191 grams (2 moles of hydroxyl groups), pay attention to heat release while stirring, and the temperature rises to 80 °C, the reaction was carried out for 3 hours. Then, 1536 grams of EDGA and 1536 grams (8 moles) of trimellitic anhydride (hereinafter referred to as TMA) were added, and the temperature was raised to 160° C. for 4 hours of reaction....
Embodiment 2
[0082] In a 20-liter flask equipped with a stirring device, a thermometer, and a condenser, add 4,300 grams of EDGA, and 2,070 grams of IPDI-N (9 moles of isocyanate groups), and isocyanates derived from 1,6-hexamethylene diisocyanate 550 g of polyisocyanic acid with urate ring (22.9% isocyanate group content, 63.3% triisocyanate content with isocyanurate ring) (3 moles of isocyanate group), after mixing uniformly, add POLYTAIL HA 2191 g (2 moles of hydroxyl groups), pay attention to heat release while stirring, and react for 3 hours after the temperature rises to 80°C. Then, 1536 grams (8 moles) of TMA were added, and after the temperature rose to 160° C., the reaction was carried out for 4 hours. The reaction now proceeds with foaming, and when the viscosity increases and it is difficult to stir in the system, add 2000 grams of EDGA to react, and the system becomes a light brown transparent liquid to obtain a polyimide resin solution.
[0083] As a result of measuring the i...
Embodiment 3
[0085] In a 20-liter flask equipped with a stirring device, a thermometer, and a condenser, add IDGA 5310 grams, and EPDI-N 1380 grams (6 moles of isocyanate groups), and isocyanates derived from norbornene diisocyanate Polyisocyanate with urate ring (isocyanate group content 18.75%, isocyanurate ring-containing triisocyanate content 65.5%) 1344 g (isocyanate group 6 moles), heated at 80°C to dissolve, then add POLYTAIL 2191 g of HA (2 moles of hydroxyl groups) was reacted at 80° C. for 5 hours while stirring, then 1,536 g (8 moles) of TMA was added, and the temperature was raised to 170° C., followed by reaction for 4 hours. The reaction proceeds together with foaming, and the system becomes a light brown transparent liquid to obtain a polyimide resin solution.
[0086] The result of infrared absorption spectrum was measured similarly to Example 1 using the prepared polyimide resin solution. 2,270cm that is characteristic absorption of isocyanate -1 Completely disappeared, ...
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