Synthesis and purification method of high-purity N-isobutoxy methacrylamide (IBMA)

[0029] Example 1: This embodiment provides a synthesis and purification method of high pure-grade N-isobutyoxymethyl acrylamide IBMA, including the following steps:

[0030] S1: 350 ml of anhydrous ethanol was added to a 500 ml round bottom flask, and a tetramethyl chloride 11g (0.1 mol) was added, 5.2 g of sodium hydroxide was added, and the heating was refluxed for 4 hours, cooled to room temperature, and the precipitate was separated from centrifugation , Take the supernatant 200ml. Add about 200 g of baked activated trioxide (α-al) to the supernatant 2 O 3 ), To ensure that the aluminum diameters are all immersed in a solution, and the room temperature is allowed to stand for 24 hours. The mesoporous alumina was filtered, and the nitrogen gas was purged to dry, and the loaded quaternary alkali catalyst was stored, stored in a vacuum dryer, spare, the resulting catalyst was calculated as CAT ME 4 NOH / AO.

[0031] S2: In the 500ml round bottom flask, add 120g Cat ME 4 NOH / AO, add 110 mL of deionized water, adding 7.5 g (0.06 mol) of methoxyphenol, 600 g (8.45 mol) and isobutanol 608g (8.2 mol), and the system temperature gradually increased to the system temperature. 65 ° C, mechanical stirring until acrylamide is all dissolved, and multiple polyoxymethylene 240 g (8 mol) is added to the system. After the addition is completed, the reaction was reacted at 68 to 70 ° C for 3 hours, and then the catalyst in the system was lowered by gauze, and the mesoporous alumina was carefully washed with a small amount of deionized water (50 mL) to give N-isobutyl oxygen. The filtrate of primary acrylamide;

[0032] S3: The resulting filtrate was added a small amount of 1 M dilute sulfuric acid (about 10 mL) to regulate the system pH to 7.5 to 8.0. Transferring the reaction liquid to the short-range molecular distiller, distilled at 70 ° C for 4 hours. The product was collected from the discharge tube located at the bottom of the evaporator to give crystal 630 g, which is the colorless transparent N-isobutyl oxygen acrylamide liquid.

[0033] The rate of reaction was 94.37%, tested, purity of 98.3%, water content of 0.3%, formaldehyde residue 122 ppm, isobutanol residue 215 ppm.

[0034] Example 2

[0035] S1: 350 ml of anhydrous ethanol was added to a 500 ml round bottom flask, and tetrabutylammonium bromide was added 15 g (0.1 mol), 11.2 g of potassium hydroxide, and heated and refluxed for 4 hours, cooled to room temperature, centrifugation , Take the supernatant 200ml. To the supernatant, about 200 g of baked activated tri-aluminum (α-Al2O3) was added to ensure that the aluminum dioxide was immersed in a solution, and the room temperature was allowed to stand for 24 hours. The mesoporous alumina was filtered, and the nitrogen gas was purged to dry, and the loaded quaternary amine catalyst was stored, stored in a vacuum dryer, and the resulting catalyst was recorded as CAT bu 4NOH / AO..

[0036] S2: In a 500 ml round bottom flask, 150 g of Cat Bu4NOH / AO was added, and 170 g of deionized water was added, and the addition of benzene phenol 4.4 g (0.04 mol), acrylamide 574 g (8 mol) and isobutanol (8.1). Mol), the system temperature gradually warmed to 50 ° C, mechanically stirred all of the acrylamide, and added multiplexaldehyde 230 g (7.67 mol) in the batch to the system. After the addition was completed, at 50 ° C for 6 hours, then heat the meter alumina in the system was filtered off, and the mesoporous alumina was carefully washed with a small amount of deionized water (30 mL).

[0037] S3: The resulting filtrate was added a small amount of 1 M dilute hydrochloric acid (about 8 mL) to regulate the pH of 7.5 to 8.0. Transferring the reaction liquid to the short-range molecular distiller, distilled at 70 ° C for 4 hours. The product was collected from the discharge tube located at the bottom of the evaporator to obtain a crystal 630 g, the resulting colorless transparent N-isobutylmethylacrylamide liquid.

[0038] The rate of reaction was 96.67%, tested, purity was 98.9%, and the moisture content was 0.2%, formaldehyde residue 96 ppm, isobutanol residue 163 ppm.