Curable amine flux composition and method of soldering
A technology of flux and composition, which is applied in chemical instruments and methods, preparation of organic compounds, preparation of amino hydroxyl compounds, etc., and can solve problems such as reducing the reliability of product equipment
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Embodiment 1
[0054] Embodiment 1: the synthesis of amine flux
[0055] The 2,6-diamino-2,5,6-trimethylheptan-3-olamine flux was prepared by the following method. First, the following synthetic method was used to prepare 2,5,6-trimethyl-2,6-dinitroheptan-3-ol intermediate
[0056]
[0057] Specifically, a stirring bar, a pair of thermocouples, a dropping funnel with a nitrogen inlet and a lid for a condenser were installed in a three-necked round bottom flask. The flask was then charged with 2-nitropropane (50 g, 0.56 mol, 5.0 equiv) and a catalytic amount of 1,8-diazabicyclo[5.4.0]undec-7-ene. The contents of the flask were then stirred under nitrogen for 30 minutes. Crotonaldehyde (7.9 g, 9.2 mL, 0.112 mol, 1.0 equiv) was then added dropwise to the flask over twenty minutes. The contents of the flask were then stirred under nitrogen for 5-6 hours, during which time a white solid was observed to precipitate out of solution. At this point, GC analysis showed the absence of any croton...
Embodiment 2
[0061] Embodiment 2: the synthesis of amine flux
[0062] 2,6-diamino-2,6-dimethyl-5-phenylheptan-3-olamine flux was prepared by the following method. First, 2,6-dimethyl-2,6-dinitro-5-phenylheptan-3-ol intermediate was prepared by the following synthetic method
[0063]
[0064] Specifically, a stirring bar, a pair of thermocouples, a dropping funnel with a nitrogen inlet and a lid for a condenser were installed in a three-necked round bottom flask. The flask was then charged with 2-nitropropane (101.1 g, 1.14 mol, 6.0 equiv) and a catalytic amount of 1,8-diazabicyclo[5.4.0]undec-7-ene ("DBU"). The contents of the flask were then stirred under nitrogen for 20 minutes. Trans-cinnamaldehyde (25.0 g, 0.19 mole, 1.0 equiv) was then added dropwise to the flask over twenty minutes. During the dropwise addition of trans-cinnamaldehyde, an exotherm of approximately 22°C was observed. After complete addition of trans-cinnamaldehyde, the contents of the flask were heated to 50°C...
Embodiment 3
[0068] Embodiment 3: the synthesis of amine flux
[0069] Amine fluxes with the following structure
[0070]
[0071] Prepared by the following method. Specifically, the product of Example 1 (0.05 mol) was added to a reaction vessel with a stirrer bar. The reactor was then placed on a heating mantle with magnetic stirring. The reaction vessel was then inertized with nitrogen, and (0.1 mol) 2-ethylhexyl glycidyl ether (supplied by Momentive Performance Materials) was then added to the reaction vessel at ambient temperature with stirring. The set temperature of the heating mantle was then raised to 75°C and the contents of the reaction vessel were allowed to continue stirring for two (2) hours. The set temperature of the heating mantle was then increased to 140°C and the contents of the reaction vessel were allowed to stir for an additional two (2) hours. The set temperature of the heating mantle was then lowered to 80°C and the reaction vessel was evacuated, reducing the...
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