N,N'-Methylenebisacrylamide synthesis
- Product Name:N,N'-Methylenebisacrylamide
- CAS Number:110-26-9
- Molecular formula:C7H10N2O2
- Molecular Weight:154.17
Yield:110-26-9 87.54%
Reaction Conditions:
with dmap;1-ethyl-(3-(3-dimethylamino)propyl)-carbodiimide hydrochloride;hydroquinone in water at 65 - 75; for 2.5 h;Reagent/catalyst;Temperature;
Steps:
1-2 Example 2
The synthesis method of N,N'-methylenebisacrylamide in this embodiment includes the following steps: Add 250ml of 6wt% phosphomolybdic acid solution to a 500mL round bottom flask, and then add about 200g of activated MCM-41 molecular sieve to ensure that the molecular sieve is completely immersed in the solution. Heat to reflux for 4 hours, cool to room temperature, and stand for 12 hours Afterwards, the molecular sieve was filtered out and dried in an oven at 110 degrees for 3 hours. The resulting catalyst is designated Cat HPM/MCM. In a 250mL round bottom flask, add 20g Cat HPM/MCM and 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride 38g (0.2moL), 4-dimethylaminopyridine 24g (0.2moL), add 200ml deionized water, add 2.2g (0.02moL) hydroquinone, 287g (4moL) of acrylamide to the system, mechanically stir at room temperature, add 117g (3.92) paraformaldehyde to the system in batches moL).After the addition, the temperature of the system was gradually raised to 75°C, reacted at 75°C for 0.5 hours, then slowly cooled to 65°C, and the clinker was kept warm for 2 hours until the reaction was complete. Then 150 mL of 65°C deionized water was added to the system, and then the silica microspheres in the system were filtered off with gauze while it was hot, and the silica microspheres were carefully washed with a small amount of 65°C deionized water (about 25 mL). The obtained filtrate was carefully concentrated in vacuum to about 200 mL (60°C, 80mmHg), poured into a crystallization kettle, slowly cooled to 5°C, and allowed to stand for 24 hours to crystallize. The crystals in the centrifugal separation system were air-dried at room temperature to obtain 540 g of crystals, and the recovery rate of the obtained crystals was 87.54%.
References:
CN112679376,2021,A Location in patent:Paragraph 0032-0040
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107-06-2
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