67874-34-4Relevant articles and documents
Preparation method of diacetone acrylamide
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Paragraph 0016; 0022-0027, (2018/02/03)
The invention discloses a preparation method of diacetone acrylamide. The preparation method comprises the following steps: (1) acetone and propenenitrile are mixed and are added to concentrated sulfuric acid, acetone and propenenitrile and concentrated sulfuric acid undergo condensation reaction fully, and after the reaction is finished, a mixture is obtained; (2) the mixture is washed with a dispersing agent, after the washing is finished, solid-liquid separation is carried out, and an intermediate product is obtained; (3) the intermediate product is mixed in an organic solvent, then alkali is added, alkali and the intermediate product react in a liquid phase system, the reaction is finished when a ph value of the liquid phase system is greater than or equal to 7, and after the reaction is finished, the organic solvent in which products are dissolved is separated out, and a product solution is obtained; and (4) a polymerization inhibitor is added to the product solution, reduced pressure distillation is carried out for recovering the organic solvent, then rectification is carried out, and a fraction obtained through the rectification is diacetone acrylamide. According to the preparation method, an intermediate of diacetone acrylamide is separated out, the impurities like acrylamide and vinyl monomers can be removed, the impurity content in subsequent separation steps is few, and the content of diacetone acrylamide can be raised.
Process for preparing N-(1,1-dimethyl-3-oxobutyl)acrylamide from a 2-vinyl-1,3(4H)oxazine sulfate
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, (2008/06/13)
A process is disclosed for preparing N-(1,1-dimethyl-3-oxobutyl)acrylamide which comprises (1) contacting a dispersion of 5,6-dihydro-6-hydroxy-4,4,6-trimethyl-2-vinyl-1,3,3(4H)-oxazine-3-ium sulfate (1:1) in a water-immiscible organic solvent with a neutralizing or alkalizing amount of gaseous ammonia at a temperature between about 10° C. and 25° C. to form a solution of diacetone acrylamide in said organic solvent and a precipitate of crystalline ammonium sulfate; (2) separating the crystals of ammonium sulfate; (3) cooling the organic mother liquors recovered from step (2) to about -10° C. to 20° C. to crystallize N-(1,1-dimethyl-3-oxobutyl)acrylamide therefrom; and (4) recovering the crystals of N-(1,1-dimethyl-3-oxabutyl) acrylamide, washing the recovered crystals with a cold water-immiscible organic solvent and drying the same.