Abstract: The present disclosure relates to a method for preparing isophorone diamine by means of a hydrogenation reduction of isophorone nitrile imine. The hydrogenation reduction is continuously carried out in a multi-stage bubble column reactor loaded with a supported alkaline cobalt-based catalyst, wherein isophorone nitrile imine is successively in countercurrent contact with hydrogen in each stage of the reactor to carry out a hydrogenation reduction reaction, so as to obtain the isophorone diamine. The preparation method solves the problem of back-mixing, and further improves the conversion rate and the cis/trans ratio of the product.
Type:
Grant
Filed:
November 30, 2018
Date of Patent:
November 23, 2021
Assignees:
Zhejiang Nhu Company Ltd., Zhejiang University, Shandong Nhu Amino Acid Co., Ltd., Shandong Nhu Fine Chemical Science and Technology Company Ltd.
Abstract: Provided by the present disclosure are a method and a device for preparing 2-hydroxy-4-methylthiobutyric acid and intermediates thereof; the intermediates for preparing 2-hydroxy-4-methylthiobutyric acid comprise 3-methylthiopropionaldehyde and 2-hydroxy-4-methylthiobutyronitrile. The method for preparing 2-hydroxy-4-methylthiobutyric acid provided by the present disclosure comprises: step (1), a step of reacting acrolein with methyl mercaptan to prepare 3-methylthiopropionaldehyde; step (2), a step of reacting 3-methylthiopropionaldehyde with hydrocyanic acid to prepare 2-hydroxy-4-methylthiobutyronitrile; and step (3), a step of hydrating 2-hydroxy-4-methylthiobutyronitrile by using sulfuric acid and then hydrolyzing to prepare 2-hydroxy-4-methylthiobutyric acid; wherein in steps (1), (2) and (3), the reaction status of the materials is detected online, and the proportions of the materials are controlled according to the detection results such that reactions are performed completely.
Abstract: Provided by the present disclosure are a method and a device for preparing 2-hydroxy-4-methylthiobutyric acid and intermediates thereof; the intermediates for preparing 2-hydroxy-4-methylthiobutyric acid comprise 3-methylthiopropionaldehyde and 2-hydroxy-4-methylthiobutyronitrile.
Abstract: The present invention discloses a clean method for preparing a D,L-methionine comprising the steps of: preparing a potassium cyanide solution using a crystallized mother solution containing potassium carbonate as an absorbing liquid to absorb hydrocyanic acid, then reacting the potassium cyanide solution with 3-methylthio propionaldehyde and an ammonium bicarbonate solution at 50-150° C. for 3-15 minutes so as to obtain a 5-(?-methylthioethyl)glycolyurea solution, then bring the 5-(?-methylthioethyl)glycolyurea solution to a temperature of 140-220° C. and subjecting to a saponification reaction for 2-5 minutes, after the completion of the saponification, reducing the temperature to 0-40° C., extracting with an organic solvent, neutralizing the water phase with CO2 and crystallizing, then filtering, washing, and drying to obtain an acceptable D,L-methionine product; bring the crystallized D,L-methionine mother solution from filtration to a temperature to 110-160° C.