Ch-acidic methacrylic esters for the preparation of aqueous polymer dispersions
A technology of methyl and compound, which is used in the field of CH-acid methacrylate for preparing water-based polymer dispersions, can solve the problems of inapplicability, and achieve the effects of low viscosity, high storage stability and long shelf life
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Embodiment 1
[0153] Embodiment 1: Preparation N-(2-ethylamino)-2-cyanoacetamide
[0154] Initially 600 g (10.0 mol) of ethylenediamine was charged to a 2 liter four necked round bottom flask equipped with saber stirrer, stirrer motor, thermometer and 500 ml addition funnel. 248 g (2.5 mol) of methyl cyanoacetate were metered dropwise therein within 60 minutes, such that the reaction temperature did not exceed 30° C. During this time, the four-necked round-bottom flask was cooled in an ice-water bath. During the addition of methyl cyanoacetate, the reaction mixture gradually turned pink, and then lavender. To complete the reaction, the reaction mixture was stirred at room temperature for an additional 90 minutes.
[0155] Subsequently, excess ethylenediamine was removed under reduced pressure. For this purpose, the reaction mixture was heated to 100° C. (oil bath temperature) and the volatile constituents were distilled off at a pressure of up to 5 mbar over a period of 2 hours.
[0156...
Embodiment 2
[0160] Embodiment 2: Preparation of N-(2-cyanoethylamidoethyl) methacrylamide
[0161] A mixture of 147 g (1.2 mol) of N-(2-ethylamino)-2-cyanoacetamide and 600 g (6.0 mol) of methyl methacrylate was initially charged into a 1 liter four-neck round bottom flask with Air inlet, saber stirrer, stirrer motor and 50cm long, 29mm thick mirrored column with random packing packed with 6x6 Raschig rings. Add 7 mg (10 ppm) 4-hydroxyl-2,2,6,6-tetramethylpiperidinyl-1-oxyl group and 0.15 g (200 ppm) hydroquinone monomethyl ether to it, then add 7.4 g containing 65.6 A mixture of weight percent dioctyltin oxide and 34.4 weight percent tetraisopropyl titanate.
[0162] The reaction mixture is heated under reflux, the methanol formed being distilled off as an azeotrope via a column with random packing. After about 3.5 hours, the conversion by GC was 58%.
Embodiment 3
[0163] Example 3: Preparation of N-(2-cyanoethylamidoethyl)methacrylamide In a 2-liter three-necked round-bottomed flask, 312 g (2.4 mol) of N-(2-ethanediol) obtained from Example 1 Amino)-2-cyanoacetamide was dissolved in 468 g of water in a flask equipped with saber stirrer, stirrer motor, thermometer and 500 ml addition funnel. Thereto, 370 g (2.4 mol) of methacrylic anhydride were slowly added dropwise, whereupon a pale brown precipitate formed. The reaction mixture was then stirred for a further 1.5 hours at 80°C.
[0164]The resulting clear dark red reaction mixture was freed of low boilers under reduced pressure, concentrated to 646 g, and 400 g of isopropanol were added thereto. This resulted in the formation of a precipitate which was isolated by filtration.
[0165] The product was obtained as a brown crystalline solid with a purity of 95.0 area % (determined using GC-RV). Product yield was 346 g (73.9%).
[0166] The solubility of the product in water was determ...
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Abstract
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