Low pressure process for manufacture of 3-dimethylaminopropylamine (DMAPA)
View Patent ↗An improved process for the production of 3-dimethylaminopropylamine in high purity from N,N-dimethylaminopropionitrile utilizing a low pressure hydrogenation process is described. The basic process comprises contacting the nitrile with hydrogen at low pressure in the presence of a catalyst under conditions sufficient to effect the conversion of the nitrile to the primary amine product.
1. A process for the production of N,N-dimethylaminopropylamine from N,N-dimethylaminopropionitrile by low pressure hydrogenation comprising:
feeding hydrogen and N,N-dimethylaminopropionitrile into a low-pressure reactor containing a sponge nickel catalyst, at least one Group IA alkali metal hydroxide, and water to form a reaction medium;
heating the reaction medium to a temperature of about 70° C. to about 100° C.;
pressurizing the reactor to a pressure of about 45 psig to about 500 psig;
mixing the reaction medium; and
hydrogenating the nitrile to form N,N-dimethylaminopropylamine.
2. The process of claim 1 , wherein the selectivity of N,N-dimethylaminopropionitrile to N,N-dimethylaminopropylamine is greater than about 99.60%.
3. The process of claim 1 , wherein the selectivity of N,N-dimethylaminopropionitrile to N,N-dimethylaminopropylamine is greater than about 99.90%.
4. The process of claim 1 , wherein the Group IA alkali metal hydroxide is selected from the group consisting of sodium hydroxide, potassium hydroxide, rubidium hydroxide, cesium hydroxide and mixtures thereof.
5. The process of claim 1 wherein the Group IA alkali metal hydroxide is potassium hydroxide.
6. The process of claim 1 wherein the Group IA alkali metal hydroxide is sodium hydroxide.
7. The process of claim 1 wherein the Group IA alkali metal hydroxide is a mixture of sodium hydroxide and potassium hydroxide.
8. The process according to claim 1 wherein the temperature is between 85° C. and 95° C.
9. The process of claim 1 wherein the pressure is between 45 psig and 300 psig.
10. The process of claim 1 wherein the pressure is between 45 psig and 150 psig.
11. The process of claim 1 wherein the pressure is between 45 psig and 110 psig.
12. The process of claim 1 wherein the amount of water is about 0.1 wt. % to about 10 wt. % of the reaction medium.