The purpose of the invention is to provide a program speed temperature control the preparation of high purity anhydrous praseodymium chloride or neodymium chloride, the method in the industrial scale of high purity anhydrous praseodymium chloride or neodymium chloride products, including water content is less than 0. 1%, the product is added to water dissolved immediately, dissolved after solution clear transparent, product purity is more than 99%, the yield more than 99%. Technical solutions will directly out of the rare earth extraction separation, preparation of praseodymium chloride or neodymium chloride solution concentration crystal, get granular crystal PrCl3, BH2O or NdCl3, 6 h20, using rare earth oxide flowmeter with praseodymium oxide or neodymium oxide purity is more than 99. 9%, PrCl3 · 6 Η 20 or NdCl3 · Η 20 and ammonium chloride by weight than 2 1 mixture in the mixer, the materials are available to the mixture to the volume of 1 liter porcelain bowl, then put porcelain bowl containing material evenly to the program in the heating furnace, water injection pump pumping air into vacuum state, When the vacuum degree reaches 0. OSPA, the heating procedure is set to start heating. The heating procedure is 150°C at room temperature, the heating rate is 1. 080C/min, the heating time is 2 hours, and the holding time is 2 hours at 150°C. 150°C 240°C, the heating rate is 0. 750C/min, the heating time is 2 hours, the holding time is 4 hours; 240°C 300°C, heating rate of 0.5 °C/min, heating time of 2 hours, at 300°C holding time of 2 hours; 300 ° C to 350 ° C, the heating rate of 0. 420 C/min, heat for 2 hours, at 350 ° C holding time 6. 5 6. 8 hours, furnace temperature natural down to 50 ° C, discharging, vacuum packaging, anhydrous praseodymium chloride or neodymium chloride by the analysis of testing water content is less than 0. 1%, join immediately dissolved in water, dissolved after solution clear transparent, product purity is more than 99. 9%. Invention effect dehydration temperature in the present invention is the preparation of high purity anhydrous praseodymium chloride or neodymium chloride is the most key factors, using temperature programmed control furnace materials in the same temperature dehydration, rc, control temperature changes due to the heating system belongs to the external heated heating, heating up too fast or holding time is short, to the internal temperature of the furnace body is not even, can cause high temperature hydrolysis easily happened near the furnace material, generate ftoci or NdOCl, low and middle temperature, material dehydration is incomplete, the anhydrous chloride praseodymium and neodymium chloride in water insolubles and water content on the high side, so let’s set up strict and segmented heat preservation time. The low addition amount of ammonium chloride is easy to generate FTOCl or NDOCL, the high addition amount of ammonium chloride is high, the cost is high, and at the same time, trace impurities in ammonium chloride will be enriched in the product, affecting the product quality. This technology is applied in the industrial scale programmable heating furnace to produce 90kg praseodymium chloride anhydrous or neodymium chloride for each batch. The moisture content of the obtained praseodymium chloride anhydrous or neodymium chloride is less than 0.1%, which is immediately dissolved in water, and the aqueous solution is clear and transparent after dissolution.
Concrete implementation way of case example 1130 kg PrCl3 · 6 h20 crystals and 65 kg ammonium chloride crystals in a mixing machine mixing, materials are available to the mixture to porcelain bowl, then put porcelain bowl containing material evenly to the program in the heating furnace, water also vacuum pump pumping air into vacuum state, when the vacuum degree reaches 0. 08, set the temperature program began to heat, temperature program for room temperature of 150 ° C, heating rate of 1. 8 ° C/min, heat for 2 hours, 2 hours at 150 ° C heat preservation time; 150°C 240°C, the heating rate is 0. 75 V/min, the heating time is 2 hours, the holding time is 4 hours at 240 V; 240 V 300 V, heating rate of 0.5 °C/min, heating time of 2 hours, at 300°C holding time of 2 hours; 300 ° C to 350 ° C, the heating rate of 0. 42 ° C/minutes, the heating time 2 hours, at 350 ° C holding time 6. 5 hours, furnace temperature natural down to 50 ° C, discharging, vacuum packaging, get 90. 4 kg of anhydrous praseodymium chloride, by the analysis of testing water content is 0. 05%, join immediately dissolved in water, dissolved after solution clear transparent, anhydrous praseodymium chloride purity is 99. 9%. Example 2130 kgndcl3 · 6 h20 crystals and 65 kg ammonium chloride crystals in a mixing machine mixing, materials are available to the mixture to porcelain bowl, then put porcelain bowl containing material evenly to the program in the heating furnace, water also vacuum pump pumping air into vacuum state, when the vacuum degree reaches 0. OSPa, set the temperature program began to heat, temperature program for room temperature of 150 ° C, a speed of 1.08 ° C per minute, heat for 2 hours, 2 hours at 150 ° C heat preservation time; 150°C 240°C, the heating rate is 0. 750C/min, the heating time is 2 hours, and the holding time is 4 hours at 240°C; 240°C 300°C, heating rate of 0.5 °C/min, heating time of 2 hours, at 300°C holding time of 2 hours; 300 ° C to 350 ° C, the heating rate of 0. 42 v/minutes, the heating time of 2 hours, the 350 v holding time 6. 6 hours, furnace temperature natural down to 50 ° C, discharging, vacuum packaging, get 90. 6 kg of anhydrous neodymium chloride by the analysis of testing water content is 0. 06%, join immediately dissolved in water, dissolved after solution clear transparent, anhydrous neodymium chloride purity is 99. 9%. Implementation example 3 130 kg NdCl3 · 6 h20 crystals and 65 kg ammonium chloride crystals in a mixing machine mixing, materials are available to the mixture to porcelain bowl, then put porcelain bowl containing material evenly to the program in the heating furnace, water also vacuum pump pumping air into vacuum state, when the vacuum degree reaches 0. 08, set the temperature program began to heat, temperature program for room temperature of 150 ° C, heating rate of 1. 8 ° C/min, heat for 2 hours, 2 hours at 150 ° C heat preservation time; 150°C 240°C, the heating rate is 0. 75 V/min, the heating time is 2 hours, the holding time is 4 hours at 240 V; 240 V 300 V, heating rate of 0.5 °C/min, heating time of 2 hours, at 300°C holding time of 2 hours; 300 ° C to 350 ° C, the heating rate of 0. 42 ° C/minutes, the heating time 2 hours, at 350 ° C holding time 6. 8 hours, furnace temperature natural down to 50 ° C, discharging, vacuum packaging, get 90. 7 kg of anhydrous neodymium chloride by the analysis of testing water content is 0. 05%, join immediately dissolved in water, dissolved after solution clear transparent, anhydrous neodymium chloride purity is 99. 9%.
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