Applied Chemistry This document is the property of NECSA and shall not be used, reproduced, transmitted or disclosed without prior written permission CONCISE PROCESS DESCRIPTION OF THE BATCH BENCH SCALE PHOSPHOROUS PENTAFLUORDIE AND LITHIUM HEXAFLUOROPHPOSPHATE PILOT PLANTS DOC NO: AC-LIPF6TECH-DES-20006 Revision: 1 Author: HF Niemand and I Govender 24 August 2020 The electronic version of this document within the DocMan System is regarded as the official document Page 1 of 4 Last printed 2020/12/14 12:15:00 OPEN Applied Chemistry TABLE OF CONTENTS 1 Purpose and Scope .......................................................................................................................... 3 2 CONCISE PROCESS DESCRIPTION OF THE BATCH BENCH SCALE PHOSPHOROUS PENTAFLUORIDE PILOT PLANT ............................................................................................................................................. 3 2.1 BLOCK FLOW DIAGRAM..................................................................................................................... 3 2.2 PROCESS DESCRIPTION ...................................................................................................................... 3 3 CONCISE PROCESS DESCRIPTION OF THE BATCH BENCH SCALE LITHIUM HEXAFLUOROPHOSPHATE PILOT PLANT ............................................................................................................................................. 4 3.1 BLOCK FLOW DIAGRAM..................................................................................................................... 4 3.2 PROCESS DESCRIPTION ...................................................................................................................... 4 AC-LIPF6TECH-DES-20006 Rev: 1 Page 2 of 4 Last printed 2020/12/14 12:15:00 OPEN Applied Chemistry 1 Purpose and Scope This document contains a concise process description for a batch bench scale pilot plant for the production of lithium hexafluorophosphate. The pilot plant consists of two sections: (1) The reaction of phosphorus pentoxide, sodium fluoride and anhydrous hydrogen fluoride to produce phosphorous pentafluoride, and (2) the reaction of phosphorous pentafluoride from the first section with lithium fluoride to form lithium hexafluorophosphate. 2 CONCISE PROCESS DESCRIPTION OF THE BATCH BENCH SCALE PHOSPHOROUS PENTAFLUORIDE PILOT PLANT 2.1 BLOCK FLOW DIAGRAM Phosphorus pentoxide Anhydrous Phosphorus hydrogen fluoride pentafluoride to lithium Dissolution Reaction Crystallization Filtration Drying Decomposition Sodium hexafluoro phosphate fluoride pilot plant Sodium fluoride Recovered hydrogen fluoride Distillation Recovered sodium acid fluoride liquor Aqueous Evaporation hydrogen fluoride 2.2 PROCESS DESCRIPTION The process is a batch process. Sodium fluoride is dissolved in an excess of anhydrous hydrogen fluoride. The solution reacts with phosphorous pentoxide to form sodium hexafluoro phosphate. After evaporation of some of the excess hydrogen fluoride, the sodium hexafluoro phosphate is crystallized and the crystals are separated from the liquor by filtration. The crystals are dried at an elevated temperature. The dry crystals are decomposed at an elevated temperature to form phosphorous pentafluoride gas and sodium fluoride. The sodium fluoride is recycled for dissolution. The phosphorous pentafluoride gas is captured by freezing, thawed and stored for usage by the lithium hexafluoro phosphate pilot plant. The filtrate from the filter is distilled to recover most of the excess hydrogen fluoride. The recovered hydrogen fluoride is recycled to the dissolution reactor. The excess water in the bottom product is evaporated and the remaining sodium acid fluoride liquor is recycled to the dissolution reactor. AC-LIPF6TECH-DES-20006 Rev: 1 Page 3 of 4 Last printed 2020/12/14 12:15:00 OPEN Applied Chemistry 3 CONCISE PROCESS DESCRIPTION OF THE BATCH BENCH SCALE LITHIUM HEXAFLUOROPHOSPHATE PILOT PLANT 3.1 BLOCK FLOW DIAGRAM Phosphorous pentafluoride Anhydrous Hydrogen fluoride Lithium Dissolution Reaction Crystallization Filtration Drying Lithium fluoride hexafluorophosphate Recovered hydrogen fluoride 3.2 PROCESS DESCRIPTION The process is a batch process. Lithium fluoride is dissolved in an excess of anhydrous hydrogen fluoride. The solution reacts with phosphorus pentafluoride to form lithium hexafluorophosphate. The lithium hexafluorophosphate is crystallized and the crystals are separated from the liquor by filtration. The crystals are dried at an elevated temperature. The filtrate from the filter is recycled to the dissolution reactor. AC-LIPF6TECH-DES-20006 Rev: 1 Page 4 of 4 Last printed 2020/12/14 12:15:00 OPEN .