CN102502756B - Preparation of high-purity anhydrous praseodymium chloride or neodymium chloride by programmed heating method - Google Patents
Preparation of high-purity anhydrous praseodymium chloride or neodymium chloride by programmed heating method Download PDFInfo
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- CN102502756B CN102502756B CN 201110346246 CN201110346246A CN102502756B CN 102502756 B CN102502756 B CN 102502756B CN 201110346246 CN201110346246 CN 201110346246 CN 201110346246 A CN201110346246 A CN 201110346246A CN 102502756 B CN102502756 B CN 102502756B
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Abstract
The invention relates to preparation of high-purity anhydrous praseodymium chloride or neodymium chloride by a programmed heating method, and belongs to the field of preparation of rare-earth materials. PrCl3.6H2O or NdCl3.6H2O and ammonium chloride are mixed in a weight ratio of 2:1, and vacuumizing is performed by using a water jet pump; when the vacuum degree reaches 0.08Pa, a heating program is set for heating at the temperature of between room temperature and 350 DEG C, and the sectional heating speed and the heat preservation time are controlled; by analysis and detection, the water content of the obtained anhydrous praseodymium chloride or neodymium chloride is less than 0.1 percent; and the anhydrous praseodymium chloride or neodymium chloride is immediately dissolved when added into water, the aqueous solution obtained after the anhydrous praseodymium chloride or neodymium chloride is dissolved is clear and transparent, and the purity of the product is over 99.9 percent. The method has already been applied to a production line capable of producing 90 kilograms of anhydrous praseodymium chloride or neodymium chloride in each batch in an industrial-scale programmed heating furnace.
Description
Technical field
The present invention relates to a kind of programmed temperature method and prepare high-pure anhydrous praseodymium chloride or Neodymium trichloride method, belong to the rare earth material preparation field.
Background technology
Anhydrous chlorides of rase praseodymium and Neodymium trichloride can be respectively applied for the Application Areass such as preparation of organic catalyst compound, synthetic rubber catalyzer, high-purity praseodymium or neodymium metal.Anhydrous chlorides of rase praseodymium or Neodymium trichloride preparation method have chloride monohydrate evaporation, oxide compound chlorination process and thionyl chloride evaporation etc." the NdCl that document Zhang Yifeng is shown
3-LiCl and NdCl
3The research of-LiCl-NaCl system phase diagram ", chemical journal, 1989,47 (1): 14-18. provides a kind of preparation method of anhydrous chlorides of rase neodymium, with NdCl
36H
2O places P
2O
5Preliminary hydro-extraction in the moisture eliminator, limit heating edge suction decompression in HCl atmosphere then, dehydration obtains the anhydrous chlorides of rase neodymium step by step, and this method hydrogen chloride gas in industrial-scale production is more serious to equipment corrosion, needs simultaneously tail gas is carried out intensive treatment; " the formation calculation of thermodynamics and the application of anhydrous chlorides of rase neodymium " that the document Chen Hui winter is shown, rare earth, 1989, (3): 4-7. provides a kind of preparation method of anhydrous chlorides of rase neodymium, with NH
4Cl and Nd
2O
3Mix, under vacuum condition, heat up gradually, obtain the anhydrous chlorides of rase neodymium, Nd
2O
3Chlorination rate reaches 100%; Document Zheng is towards the expensive " PrCl that shows
3-SrCl
2The research of-LiCl ternary system phasor ", Peking University's journal (natural science edition), 1989,25 (6): 658-663. provides a kind of preparation method of anhydrous chlorides of rase praseodymium, with PrCl
36H
2O reduces pressure in dry HCl atmosphere and dewaters step by step, obtains the anhydrous chlorides of rase praseodymium.These methods are not to water content and water-insoluble analysis in anhydrous chlorides of rase praseodymium or the Neodymium trichloride product, and organic catalyst compound requires the dissolving that is added to the water at once of high-pure anhydrous praseodymium chloride or Neodymium trichloride, the dissolving rear solution is limpid transparent, can not contain water-insoluble, high-pure anhydrous praseodymium chloride or Neodymium trichloride water content all require less than 0.1%.
Summary of the invention
The purpose of this invention is to provide a kind of method for preparing high-pure anhydrous praseodymium chloride or Neodymium trichloride by programmed temperature method, this method obtains high-pure anhydrous praseodymium chloride or Neodymium trichloride product in technical scale, wherein water content is less than 0.1%, product is added to the water and dissolves at once, the dissolving rear solution is limpid transparent, product purity is greater than 99%, and yield is greater than 99%.
Technical solution: will directly separate praseodymium chloride or the neodymium chloride solution heating condensing crystal of preparing, and obtain particulate state crystal PrCl from rare earth extraction
36H
2O or NdCl
36H
2O contains Praseodymium trioxide or Neodymium trioxide purity greater than 99.9% in the rare earth oxide amount, PrCl
36H
2O or NdCl
36H
2O and ammonium chloride mixed in mixer by weight 2: 1, it is in 1 liter of porcelain alms bowl that mixed material is respectively charged into volume, the porcelain alms bowl that will contain material is more evenly put in the temperature programming stove, vacuumize with water jet pump, when vacuum tightness reaches 0.08Pa, set heating schedule and begin heating, heating schedule is: room temperature～150 ℃, heat-up rate is 1.08 ℃/minute, and 2 hours heating-up times were 150 ℃ of soaking times 2 hours; 150 ℃～240 ℃, heat-up rate is 0.75 ℃/minute, and 2 hours heating-up times were 240 ℃ of soaking times 4 hours; 240 ℃～300 ℃, heat-up rate is 0.5 ℃/minute, and 2 hours heating-up times were 300 ℃ of soaking times 2 hours; 300 ℃～350 ℃, heat-up rate is 0.42 ℃/minute, 2 hours heating-up times are 350 ℃ of soaking times 6.5～6.8 hours, when furnace body temperature drops to 50 ℃ naturally, discharging, vacuum packaging, anhydrous chlorides of rase praseodymium that obtains or Neodymium trichloride detect water content by analysis less than 0.1%, and dissolving at once is added to the water, the dissolving rear solution is limpid transparent, and product purity is greater than 99.9%.
The invention effect: dehydration temperaturre is high-pure anhydrous praseodymium chloride of preparation or Neodymium trichloride most critical factor among the present invention, adopt the interior material of temperature programming control body of heater under same temperature, to dewater, controlled temperature changes ± 1 ℃, because heating member is the external-heat heating, heat-up rate is too fast or soaking time short, it is inhomogeneous to pass to the body of heater internal temperature, can cause near the body of heater temperature of charge is too high hydrolysis very easily takes place, generate PrOCl or NdOCl, and the middle part temperature is on the low side, material dewatering is incomplete, contains water-insoluble in anhydrous chlorides of rase praseodymium that obtains or the Neodymium trichloride and water content is higher, so want strict heat-up rate and the segmentation soaking time set.The ammonium chloride add-on is on the low side, generates PrOCl or NdOCl easily, and the ammonium chloride add-on is higher, and cost is higher, and simultaneously trace impurity can enrichment in product in the ammonium chloride, influences quality product.This technology is applied in every batch in plant-scale temperature programming stove and produces anhydrous chlorides of rase praseodymium or Neodymium trichloride 90kg, and high-pure anhydrous praseodymium chloride that obtains or Neodymium trichloride water content are added to the water and dissolve at once less than 0.1%, and the dissolving rear solution is limpid transparent.
Embodiment
Embodiment 1
130kg PrCl
36H
2O crystal and 65kg ammonia chloride crystal mix in mixer, mixed material is respectively charged in the porcelain alms bowl, the porcelain alms bowl that will contain material is more evenly put in the temperature programming stove, water also vacuum pump vacuumizes, and when vacuum tightness reaches 0.08Pa, sets heating schedule and begins heating, heating schedule is: room temperature～150 ℃, heat-up rate is 1.08 ℃/minute, and 2 hours heating-up times were 150 ℃ of soaking times 2 hours; 150 ℃～240 ℃, heat-up rate is 0.75 ℃/minute, and 2 hours heating-up times were 240 ℃ of soaking times 4 hours; 240 ℃～300 ℃, heat-up rate is 0.5 ℃/minute, and 2 hours heating-up times were 300 ℃ of soaking times 2 hours; 300 ℃～350 ℃, heat-up rate is 0.42 ℃/minute, and 2 hours heating-up times were 350 ℃ of soaking times 6.5 hours, when furnace body temperature drops to 50 ℃ naturally, discharging, vacuum packaging obtains the anhydrous chlorides of rase praseodymium of 90.4kg, detecting water content by analysis is 0.05%, be added to the water and dissolve at once, the dissolving rear solution is limpid transparent, and anhydrous chlorides of rase praseodymium purity is 99.9%.
Embodiment 2
130kg NdCl
36H
2O crystal and 65kg ammonia chloride crystal mix in mixer, mixed material is respectively charged in the porcelain alms bowl, the porcelain alms bowl that will contain material is more evenly put in the temperature programming stove, water also vacuum pump vacuumizes, and when vacuum tightness reaches 0.08Pa, sets heating schedule and begins heating, heating schedule is: room temperature～150 ℃, heat-up rate is 1.08 ℃/minute, and 2 hours heating-up times were 150 ℃ of soaking times 2 hours; 150 ℃～240 ℃, heat-up rate is 0.75 ℃/minute, and 2 hours heating-up times were 240 ℃ of soaking times 4 hours; 240 ℃～300 ℃, heat-up rate is 0.5 ℃/minute, and 2 hours heating-up times were 300 ℃ of soaking times 2 hours; 300 ℃～350 ℃, heat-up rate is 0.42 ℃/minute, 2 hours heating-up times are 350 ℃ of soaking times 6.6 hours, when furnace body temperature drops to 50 ℃ naturally, discharging, vacuum packaging, it is 0.06% that the anhydrous chlorides of rase neodymium that obtains 90.6kg detects water content by analysis, dissolving at once is added to the water, the dissolving rear solution is limpid transparent, and anhydrous chlorides of rase neodymium purity is 99.9%.
Embodiment 3
130kg NdCl
36H
2O crystal and 65kg ammonia chloride crystal mix in mixer, mixed material is respectively charged in the porcelain alms bowl, the porcelain alms bowl that will contain material is more evenly put in the temperature programming stove, water also vacuum pump vacuumizes, and when vacuum tightness reaches 0.08Pa, sets heating schedule and begins heating, heating schedule is: room temperature～150 ℃, heat-up rate is 1.08 ℃/minute, and 2 hours heating-up times were 150 ℃ of soaking times 2 hours; 150 ℃～240 ℃, heat-up rate is 0.75 ℃/minute, and 2 hours heating-up times were 240 ℃ of soaking times 4 hours; 240 ℃～300 ℃, heat-up rate is 0.5 ℃/minute, and 2 hours heating-up times were 300 ℃ of soaking times 2 hours; 300 ℃～350 ℃, heat-up rate is 0.42 ℃/minute, 2 hours heating-up times are 350 ℃ of soaking times 6.8 hours, when furnace body temperature drops to 50 ℃ naturally, discharging, vacuum packaging, it is 0.05% that the anhydrous chlorides of rase neodymium that obtains 90.7kg detects water content by analysis, dissolving at once is added to the water, the dissolving rear solution is limpid transparent, and anhydrous chlorides of rase neodymium purity is 99.9%.
Claims (1)
1. one kind prepares the method for high-pure anhydrous praseodymium chloride or Neodymium trichloride by programmed temperature method, it is characterized in that, with directly separating praseodymium chloride or the neodymium chloride solution heating condensing crystal of preparing from rare earth extraction, obtains particulate state crystal PrCl
36H
2O or NdCl
36H
2O contains Praseodymium trioxide or Neodymium trioxide purity greater than 99.9% in the rare earth oxide amount, PrCl
36H
2O or NdCl
36H
2O and ammonium chloride mixed in mixer by weight 2: 1, it is in 1 liter of porcelain alms bowl that mixed material is respectively charged into volume, the porcelain alms bowl that will contain material is more evenly put in the temperature programming stove, vacuumize with water jet pump, when vacuum tightness reaches 0.08Pa, set heating schedule and begin heating, heating schedule is: room temperature～150 ℃, heat-up rate is 1.08 ℃/minute, and 2 hours heating-up times were 150 ℃ of soaking times 2 hours; 150 ℃～240 ℃, heat-up rate is 0.75 ℃/minute, and 2 hours heating-up times were 240 ℃ of soaking times 4 hours; 240 ℃～300 ℃, heat-up rate is 0.5 ℃/minute, and 2 hours heating-up times were 300 ℃ of soaking times 2 hours; 300 ℃～350 ℃, heat-up rate is 0.42 ℃/minute, 2 hours heating-up times are 350 ℃ of soaking times 6.5～6.8 hours, when furnace body temperature drops to 50 ℃ naturally, discharging, vacuum packaging, anhydrous chlorides of rase praseodymium that obtains or Neodymium trichloride detect water content by analysis less than 0.1%, and dissolving at once is added to the water, the dissolving rear solution is limpid transparent, and product purity is greater than 99.9%.
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104944459B (en) * | 2015-07-01 | 2016-08-31 | 乐山沃耐稀电子材料有限公司 | A kind of preparation method of anhydrous Neodymium chloride |
| CN106915759B (en) * | 2015-12-25 | 2019-04-09 | 中国石油天然气股份有限公司 | A kind of method that programmed temperature method prepares a Neodymium chloride hydrate |
| CN110540227A (en) * | 2018-10-29 | 2019-12-06 | 天津包钢稀土研究院有限责任公司 | Preparation method of high-quality anhydrous rare earth chloride and bromide |
| CN112010339B (en) * | 2020-09-04 | 2021-06-18 | 内蒙古蒙稀新材料有限责任公司 | Preparation method of high-purity anhydrous rare earth chloride |
| CN113072090B (en) * | 2021-04-23 | 2022-08-05 | 中国恩菲工程技术有限公司 | Preparation method of anhydrous scandium chloride molten salt |
| CN113336256B (en) * | 2021-06-17 | 2023-09-05 | 虔东稀土集团股份有限公司 | Preparation method of anhydrous rare earth neodymium chloride |
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| US2982603A (en) * | 1947-06-24 | 1961-05-02 | Kent M Harmon | Preparation of anhydrous cerium chloride, uranium bromide, or plutonium fluoride |
| SU827398A1 (en) * | 1979-02-26 | 1981-05-07 | Университет дружбы народов им.Патриса Лумумбы | Method of producing anhydrous light lanthanides tribromides |
| EP0407242A1 (en) * | 1989-06-22 | 1991-01-09 | Rhone-Poulenc Chimie | Dehydrated mixtures of rare earth halides and alkaline or alkaline-earth halides |
| CN1785814A (en) * | 2005-12-26 | 2006-06-14 | 包头市世博稀土冶金有限责任公司 | Preparation method of anhydrous cerium chloride |
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| US2982603A (en) * | 1947-06-24 | 1961-05-02 | Kent M Harmon | Preparation of anhydrous cerium chloride, uranium bromide, or plutonium fluoride |
| SU827398A1 (en) * | 1979-02-26 | 1981-05-07 | Университет дружбы народов им.Патриса Лумумбы | Method of producing anhydrous light lanthanides tribromides |
| EP0407242A1 (en) * | 1989-06-22 | 1991-01-09 | Rhone-Poulenc Chimie | Dehydrated mixtures of rare earth halides and alkaline or alkaline-earth halides |
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