Multi-functional phenolic resins
An integer, CH2-CH2-O technology, applied in ether preparation, isocyanate derivative preparation, organic chemistry, etc., can solve problems such as mold adhesion, mold dyeing, organic acid sublimation, etc.
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Embodiment 1
[0093] Embodiment 1: the preparation of methylol compound-soluble novolac (resolac) (compound 1)
[0094] About 150 grams of low molecular weight novolak and 200 grams of formalin solution (37% by weight) were mixed in a five-neck reaction flask equipped with condenser, mechanical stirrer, dropping funnel and thermometer. The reaction was started by dropwise addition of 150 ml of 10% (by weight) sodium hydroxide solution and the pH of the reaction mixture was adjusted to between pH 9-10. The reaction mixture was heated to about 65°C for 3 hours. At the end of this period, the reaction mixture was cooled and neutralized with cold (5-10° C.) sodium dihydrogen phosphate solution. The golden resin layer was separated from the reaction mixture, dissolved in ethanol, desalted, and dried over molecular sieves. The product was evaporated by rotary evaporator and dried under vacuum to obtain compound 1. The products were characterized and their curing properties studied by different...
Embodiment 2
[0095] Embodiment 2: the preparation of amino novolac compound (compound 2)
[0096] About 30.6 grams of compound 1 were mixed with 150 ml of ethanol in a one liter autoclave system from Analis (Belgium) equipped with a mechanical stirrer and operated at controlled temperature and pressure. The system was secured and connected to an ammonia cylinder. The system was flushed with N2 and mixed for 10 minutes to dissolve the compound. Ammonia gas was fed to the autoclave until the pressure reached 1.5 atmospheres. The reaction temperature was maintained at about 50-70°C for 2 hours by the cooling jacket of the autoclave. At the end of this period, the system was cooled to room temperature and flushed with N2 to remove unreacted ammonia. The white serum product was evaporated and dried under vacuum to obtain compound 2. Based on percent N content, the number of amino groups present was determined by CHN microanalysis. The CHN data show that the number of amino groups (based on...
Embodiment 3
[0097] Embodiment 3: the preparation of diethylamino derivative (compound 3)
[0098] About 45 grams of compound 1 was refluxed with 300 grams of diethylamine (DEA) for three hours. At the end of this period, the product was cooled to room temperature and unreacted DEA was extracted several times with water. The obtained oleoresin was dissolved in ethanol and dried over molecular sieves. The product was evaporated by rotary evaporator and dried under vacuum at 80 °C and 0.1 mmHg for 3 hours to obtain compound 3. The number of diethylamine groups was determined by CHN microanalysis. The number of substituted amino groups was 20-30% less than the number of methylol groups due to the catalytic polymerization of novolac in the presence of DEA. The number of DEA groups evaluated was about 5-7 groups per novolak molecule.
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