Method for carrying out surface treatment on electrolytic copper foil by virtue of high-heat-resistance organosiloxane film-forming material
An organosiloxane, film-forming material technology, applied in the direction of metal material coating process, etc., can solve the problem of inability to guarantee the dense protective layer structure of the galvanized layer, false alarms, and inability to prepare high-reliability copper foils for printed circuit boards, etc. problems, to achieve good high temperature oxidation resistance, simplify the preparation process, and reduce the cost of process management.
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Embodiment 1
[0031] Maleic anhydride structure type silicone material.
[0032]Material preparation: add 9.8g (0.1mol) maleic anhydride and 100ml dehydrated acetone to a 250ml three-necked bottle, stir and dissolve at room temperature, add 16.1g (0.1mol) hexamethyldisilamine (HMDS) dropwise, Continue to stir for 30 minutes after the addition, then drop 0.2 mol of water, and precipitates will form immediately. After the system is cooled to room temperature, filter with suction, remove water and wash the filter cake with acetone three times, and dry it to obtain a light yellow powder of maleic acid Amine 7.87g, yield 81%.
[0033] Under nitrogen atmosphere, add 9.7g (0.1mol) maleic imide and 100ml dehydrated DMSO to a 250ml three-necked flask, raise the temperature to 110°C, then add 100ml dehydrated ethanol solution containing 5.61g potassium hydroxide dropwise , a white precipitate is formed. Maintain 110°C for 90 minutes, filter while hot, wash the filter cake three times with dehydrate...
Embodiment 2
[0038] Phthalic anhydride structure type silicone material.
[0039] Material preparation: under nitrogen atmosphere, add 14.8g (0.1mol) phthalic anhydride and 150ml glacial acetic acid into a 250ml three-necked flask, and add 5.7g (0.1mol) allyl Ammonia was reacted at room temperature for 1h, and then the temperature was raised to 120°C for reflux for 3h. Stop the reaction, and after cooling to room temperature, pour it into 300ml of water, immediately a white precipitate precipitates out, filter with suction, wash the filter cake with water three times, and dry to obtain the white powder product 2-allylisoindoline-1,3 - 15.8 g of diketone, the yield is 85%.
[0040] Under nitrogen atmosphere, add 9.35g (0.05mol) 2-allylisoindoline-1,3-dione and 150ml toluene into a 250ml three-neck flask, stir to dissolve, add about 0.2ml Karstedt catalyst, activate at 50°C 30min, then add 8.2g (0.05mol) triethoxysilane, heat up to 70°C, react for 10h and evaporate the solvent to obtain of...
Embodiment 3
[0044] 1,2,3,6-tetrahydrophthalic anhydride structure type silicone material.
[0045] Material preparation: Add 15.2g (0.1mol) 1,2,3,6-tetrahydrophthalic anhydride and 150ml glacial acetic acid into a 250ml three-neck flask under ice bath conditions, then add 5.7g (0.1mol) dropwise Allyl ammonia, remove the ice bath and stir for 1 hour, then raise the temperature to 120°C and reflux for 5 hours, after cooling to room temperature, pour it into 500ml of water, a large amount of white solid precipitates, wash the filter cake with water for three times by suction filtration, and dry at 40°C After drying, 15.86 g of a white imidation product was obtained, and the yield was 83%.
[0046] Under a nitrogen atmosphere, add 8.5g (0.0445mol) of the imidation product of the previous step and 150ml of toluene to a 250ml three-neck flask, stir and dissolve and heat up to 50°C, then drop in 0.2ml of Karstedt catalyst, maintain 50°C for 30min, then drop in trimethyl Oxysilane 5.43g trimetho...
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