The present invention is directed to an improved reaction process that allows for the achievement of excellent NF₃ production yields, while minimizing the amount of unreacted fluorine exiting with the process gases and minimizing the amount of liquid melt waste (HF/NH₃) produced by the process. The basic NF₃ process resides in reacting F₂ with an ammonium ion source, e.g., ammonium acid fluoride, under conditions for forming NF₃. The improvement in the process comprises:

• introducing F₂ and said ammonium ion source cocurrently and downflow through a packed column or monolith column at a first temperature;
• reacting said F₂ and ammonium ion source in said column; and,
• removing a mixture of NF₃ and byproducts from said column at a second temperature higher than said first temperature.