Method for nitrogen trifluoride production

Abstract

A method for the production of nitrogen trifluoride from a fluorine reactant and an ammonium ion source that is dispersed within a liquid-phase reaction mixture containing one or more perfluorocarbon fluids is disclosed. In certain preferred embodiments, the fluorine reactant is introduced to the reaction mixture at a temperature that ranges from 90° C. to 120° C. In these embodiments, the percentage yield of nitrogen trifluoride is about 80% or greater.

We claim:  
     
         1 . A method for producing a nitrogen trifluoride product, the method comprising: 
 providing a reaction mixture comprising an ammonium source and a perfluorcarbon compound wherein at least a portion of the ammonium source comprises a solid; and    introducing a fluorine reactant to the reaction mixture for one or more temperatures sufficient to effect a reaction and thereby form the nitrogen trifluoride product.    
     
     
         2 . The method of  claim 1  further comprising the step of heating the reaction mixture to substantially solubilize at least a portion of the ammonium source within the perfluorocarbon fluid.  
     
     
         3 . The method of  claim 1  further comprising the step of introducing an ammonia gas into the reaction mixture.  
     
     
         4 . The method of  claim 3  wherein the reaction is performed in a continuous manner with the fluorine reactant and the ammonia gas added to the reaction mixture.  
     
     
         5 . The method of  claim 1  wherein the temperature ranges from about 60° C. to about 144° C.  
     
     
         6 . The method of  claim 5  wherein the temperature ranges from about 90° C. to about 120° C.  
     
     
         7 . The method of  claim 6  wherein the percentage yield of the nitrogen trifluoride product is about 80% or greater.  
     
     
         8 . The method of  claim 7  wherein the percentage yield of the nitrogen trifluoride product is about 90% or greater.  
     
     
         9 . The method of  claim 1  wherein the weight-to-volume ratio of the ammonium source to the perfluorocarbon fluid ranges from 4:1 to 1:2.  
     
     
         10 . The method of  claim 1  wherein the ammonium source is at least one from the group consisting of NH 3 , NH 4 F, NH 4 HF 2 , NH 4 Cl, NH 4 Br, NH 4 I, NH 4 NO 3 , (NH 4 ) 3 PO 4 , (NH 4 ) 2 SO 4 , (NH 4 ) 2 CO 3 , NH 4 HCO 3 , NH 4 HSO 4 , NH 4 OSO 2 F, NH 4 OSO 2 Cl, NH 4 OSO 2 CF 3 , NH 4 OSO 2 CH 3 , NH 4 OC(O)CF 3 , NH 4 OC(O)CH 3 , NH 4 N(SO 2 CF 3 ) 2 , NH 4 OIOF 4 , NH 4 OTeF 5 , NH 4 NO 3 , (NH 4 ) 3 PO 4 , NH 4 IO 4 , NH 4 ClO 4 , and NH 4 BrO 4 , and combinations thereof.  
     
     
         11 . The method of  claim 10  wherein the ammonium source comprises ammonium fluoride.  
     
     
         12 . The method of  claim 10  wherein the ammonium source comprises ammonium bifluoride.  
     
     
         13 . The method of  claim 1  wherein the ammonium source comprises a compound of the formula (NH 4 ) y MF z .nHF wherein M is one or more elements selected from Group 1 through Group 18 of the Periodic Table of the Elements; y is a number that ranges from 1 to 4; z is a number that ranges from 2 to 8; and n is an amount that is sufficient to maintain the compound as a liquid in the exisiting reaction conditions.  
     
     
         14 . The method of  claim 1  wherein the ammonium source comprises a compound of the formula (NH 4 ) x M y A.nHF wherein M is one or more elements selected from Group 1 through 18 of the Periodic Table of the Elements; A is an anion from the group consisting of carbonate, bicarbonate, phosphate, sulfate, nitrate, periodate, perbromate, or perchlorate; x is a number that ranges from 1 to 3; y is a number that ranges from 0 to 2; and n is an amount that is sufficient to maintain the compound as a liquid in the reaction mixture.  
     
     
         15 . The method of  claim 1  wherein the reaction mixture is agitated.  
     
     
         16 . The method of  claim 1  wherein the fluorine reactant is introduced at a rate of 40 lbs per hour or greater.  
     
     
         17 . A method for producing a nitrogen trifluoride product, the method comprising: 
 combining an ammonium source and a perfluorocarbon fluid to form a reaction mixture wherein at least a portion of the ammonium source comprises a solid;    heating the reaction mixture to substantially solubilize at least a portion of the ammonium source within the perfluorocarbon compound; and    introducing a fluorine reactant to the reaction mixture for one or more temperatures sufficient to effect a reaction and thereby form the nitrogen trifluoride product.    
     
     
         18 . The method of  claim 17  further comprising the step of introducing an ammonia gas into the reaction mixture.  
     
     
         19 . The method of  claim 17  wherein the temperature ranges from about 60° C. to about 144° C.  
     
     
         20 . The method of  claim 19  wherein the temperature ranges from about 90° C. to about 120° C.  
     
     
         21 . The method of  claim 20  wherein the percentage yield of the nitrogen trifluoride product is about 80% or greater.  
     
     
         22 . The method of  claim 21  wherein the percentage yield of the nitrogen trifluoride product is about 90% or greater.  
     
     
         23 . A method for producing a nitrogen trifluoride product at a high yield, the method comprising: 
 combining an ammonium source and a perfluorocarbon fluid to form a reaction mixture wherein the ammonium source comprises a solid;    heating the reaction mixture to substantially solubilize at least a portion of the ammonium source within the perfluorocarbon fluid; and    introducing a fluorine reactant to the reaction mixture for one or more temperatures ranging from about 90° C. to about 120° C. to effect a reaction and thereby form the nitrogen trifluoride product wherein the percentage yield of the nitrogen trifluoride product is about 80% or greater.    
     
     
         24 . The method of  claim 23  further comprising the step of introducing an ammonia gas into the reaction mixture.  
     
     
         25 . The method of  claim 24  wherein the reaction is performed in a continuous manner with the fluorine reactant and an ammonia gas added to the reaction mixture.  
     
     
         26 . The method of  claim 23  wherein the reaction mixture is agitated.  
     
     
         27 . The method of  claim 23  wherein the fluorine reactant is introduced at a rate of 40 lbs per hour or greater.