CN101037216A - Preparation technique of anhydrous lanthanum chloride by chlorination baking dehydration method - Google Patents

Preparation technique of anhydrous lanthanum chloride by chlorination baking dehydration method Download PDF

Info

Publication number
CN101037216A
CN101037216A CN 200610067759 CN200610067759A CN101037216A CN 101037216 A CN101037216 A CN 101037216A CN 200610067759 CN200610067759 CN 200610067759 CN 200610067759 A CN200610067759 A CN 200610067759A CN 101037216 A CN101037216 A CN 101037216A
Authority
CN
China
Prior art keywords
roasting
anhydrous lanthanum
lanthanum chloride
chloride
preparation
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN 200610067759
Other languages
Chinese (zh)
Inventor
陈红兵
杨培志
周昌勇
蒋成勇
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Ningbo University
Kunming Institute of Physics
Original Assignee
Ningbo University
Kunming Institute of Physics
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Ningbo University, Kunming Institute of Physics filed Critical Ningbo University
Priority to CN 200610067759 priority Critical patent/CN101037216A/en
Publication of CN101037216A publication Critical patent/CN101037216A/en
Pending legal-status Critical Current

Links

Images

Landscapes

  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)

Abstract

本发明公开了无水氯化镧的氯化焙烧脱水法制备工艺,该技术属于精细无机化学试剂制备技术领域。以LaCl3·7H2O为初始原料,采用氯化氢保护下的焙烧脱水处理进行无水氯化镧的制备。在氯化焙烧脱水处理过程中,保持通入足量干燥氯化氢气体,逐步升高焙烧温度,焙烧温度控制于200~300℃,进行5~10小时焙烧处理。此工艺能够充分有效地抑制水解反应,避免产生氯氧化镧杂质,从而制备出较高纯度的无水氯化镧,所获无水氯化镧试剂可广泛应用于金属镧的熔盐电解法生产、相关稀土材料的制备等技术领域。The invention discloses a preparation process of anhydrous lanthanum chloride by a chlorination roasting dehydration method, which belongs to the technical field of preparation of fine inorganic chemical reagents. Using LaCl 3 ·7H 2 O as the initial raw material, anhydrous lanthanum chloride was prepared by roasting and dehydration under the protection of hydrogen chloride. During the chlorination roasting and dehydration process, a sufficient amount of dry hydrogen chloride gas is kept flowing, and the roasting temperature is gradually increased, and the roasting temperature is controlled at 200-300° C., and the roasting treatment is carried out for 5-10 hours. This process can fully and effectively inhibit the hydrolysis reaction and avoid the production of lanthanum oxychloride impurities, thereby preparing anhydrous lanthanum chloride with higher purity. The obtained anhydrous lanthanum chloride reagent can be widely used in the molten salt electrolysis production of metal lanthanum , Preparation of related rare earth materials and other technical fields.

Description

The chloridizing roasting evaporation preparation technology of anhydrous lanthanum chloride
Technical field
The invention belongs to fine inorganic chemical reagent preparing technical field.Anhydrous lanthanum chloride is the fine inorganic chemical reagent that has significant application value in the rare earth material production, the invention discloses the novel process of preparation anhydrous lanthanum chloride, adopt this technology can prepare the anhydrous lanthanum chloride of higher degree, the anhydrous lanthanum chloride reagent that obtains can be widely used in the fused salt electrolysis process production of lanthanoid metal, the technical fields such as preparation of relevant rare earth material.
Background technology
Along with the development of modern new material technology, anhydrous lanthanum chloride reagent obtains more and more important use in the rare earth material field, and in the process of the relevant rare earth material of development, high-pure anhydrous Lanthanum trichloride often becomes the gordian technique condition of material preparation.Existing so far more anhydrous lanthanum chloride preparation method's research report, these preparation methods mainly contain following several: (1) decompression roasting evaporation: under reduced pressure, the roasting processed by the hydration Lanthanum trichloride is with the preparation anhydrous lanthanum chloride; (2) ammonium chloride chlorination process: generate intermediate compound 2NH by lanthanum trioxide and the reaction of excess chlorination ammonium 4ClLaCl 3, under the decompression roasting condition, make intermediate compound generation thermolysis, thereby obtain anhydrous lanthanum chloride; (3) chemical vapor transport method: in the closed system that keeps the proper temperature gradient, make lanthanum trioxide and excessive Aluminum chloride anhydrous generate gaseous state title complex LaAl in the reaction of comparatively high temps district 3Cl 12, gaseous state title complex diffusion transport gradually deposits anhydrous lanthanum chloride through decomposition reaction again to lower temperature region; (4) other chlorination process: in exhausted water reaction system, adopt tetracol phenixin steam chloride oxidation lanthanum, with the preparation anhydrous lanthanum chloride.In these preparation methods, decompression roasting evaporation and ammonium chloride chlorination process all are difficult to avoid a small amount of Lanthanum trichloride generation hydrolysis, prepared product purity is lower, the preparation process technical qualification of chemical vapor transport method and other chlorination process have relatively high expectations or the reaction process time oversize, be difficult to realize the batch preparations of anhydrous lanthanum chloride.
Because the chemical property of rare earth chloride, the Lanthanum trichloride that is obtained under wet-chemical prepares condition often forms the hydration Lanthanum trichloride, and its saturated chloride monohydrate is the LaCl that contains crystal water 37H 2O adopts the processed method its contained crystal water progressively can be removed, and is yet evaporation prepares anhydrous lanthanum chloride institute inherent technical barrier: must manage fully to suppress moisture muriate generation hydrolysis, to avoid producing Lanthanum monochloride monoxide impurity.In existing decompression roasting dehydration preparation method, reduced pressure helps realizing dewatering, but can not suppress Lanthanum trichloride generation hydrolysis reaction, thereby obtained product still contains more Lanthanum monochloride monoxide impurity.The invention provides the chloridizing roasting evaporation preparation technology of anhydrous lanthanum chloride, with LaCl 37H 2O is an initial feed; adopt the roasting processed under the dry hydrogen chloride protection to carry out the preparation of anhydrous lanthanum chloride; this technology can suppress hydrolysis reaction fully effectively, avoids producing Lanthanum monochloride monoxide impurity, thereby can prepare the anhydrous lanthanum chloride reagent of higher degree.
Summary of the invention
According to the elementary heat chemical process of hydration Lanthanum trichloride generation dehydration reaction, with LaCl 37H 2O is a raw material, adopts the chloridizing roasting evaporation to prepare anhydrous lanthanum chloride, promptly under the dry hydrogen chloride gas protection, with LaCl 37H 2O carries out roasting under proper temperature, make LaCl 37H 2O progressively sloughs contained crystal water, to obtain the anhydrous lanthanum chloride of higher degree.The basic craft course of anhydrous lanthanum chloride preparation is: with LaCl 37H 2O contains into the boat-shaped quartz glass crucibles, sends in the quartz glass tube that is installed on tube type resistance furnace, steel cylinder is adorned dry hydrogen chloride gas feed quartz glass tube, and the maturing temperature that progressively raises through 5~10 hours calcination process, makes LaCl 37H 2O progressively sloughs contained humidity; In the processed process, the hydrogen chloride tail gas that adopts the diluted sodium hydroxide solution absorption system to discharge; After the roasting dehydration finishes, feed the hydrogen chloride gas of high pure nitrogen, take out treated anhydrous powder rapidly, sealed preservation to retain in the pipe blow-through.
In above-mentioned chloridizing roasting processed technology, in order fully to suppress moisture muriate generation hydrolysis, to avoid producing Lanthanum monochloride monoxide impurity, this technology must be taked two gordian technique measures: the suitable maturing temperature of (1) control is the most important condition that suppresses hydrolysis reaction.Under the situation that satisfies the dehydration requirement, should control lower maturing temperature as far as possible, maturing temperature is controlled in 200~300 ℃ usually; (2) feeding dry hydrogen chloride gas is the prerequisite that suppresses hydrolysis reaction.Actual roasting dehydration experiment shows, only depends on the suitable maturing temperature of control, still has a small amount of LaCl 3Hydrolysis reaction takes place, and contains LaOCl impurity in the obtained product to some extent.In roasting processed process, in tube type resistance furnace, continue to feed dry hydrogen chloride gas, to suppress moisture muriate generation hydrolysis reaction fully, can obtain more satisfactory dehydrating effect, thereby prepare the anhydrous lanthanum chloride of higher degree.
With both at home and abroad the report method compare, adopt the prepared anhydrous lanthanum chloride purity of chloridizing roasting processed method than higher, this technology can be applicable to batch preparations anhydrous lanthanum chloride reagent, also can attempt being applied to prepare other light rare earths anhydrous chloride.Utilize above-mentioned dewatering processing device, can prepare nearly tens kilograms of anhydrous lanthanum chlorides at every turn.Making anhydrous lanthanum chloride through the chloridizing roasting processed is the exsiccant white powder, and the anhydrous lanthanum chloride powder is easy to the moisture absorption in air, should give sealing and preserves.
Description of drawings
Chloridizing roasting dehydration experiment equipment used as shown in Figure 1, this equipment comprises hydrogen chloride gas body source, tube type resistance furnace and device for absorbing tail gas.The hydrogen chloride gas body source is a steel cylinder dress dry hydrogen chloride, and steel cylinder is furnished with special corrosion-resistant reducing valve; Quartz glass tube is installed in the tube type resistance furnace, and pending raw material splendid attire is put into the quartz glass tube middle part in the boat-shaped quartz crucible; Pipeline junction keeps good resistance to air loss, and device for absorbing tail gas is used for the hydrogen chloride tail gas that absorption system is discharged.In chloridizing roasting processed process, by polyfluortetraethylene pipe gas continue is fed tube type resistance furnace, the water vapor of deviating from from moisture muriate condensation and splash into the glass surge flask gradually, hydrogen chloride tail gas then enters sodium hydroxide solution and is absorbed.
Embodiment
Embodiments of the invention are listed below:
(1) with 1000g LaCl 37H 2O contains into the boat-shaped quartz glass crucibles, is positioned over the middle part of quartz glass tube in the tube type resistance furnace; Connect whole breather line system, feed the resistance to air loss of high pure nitrogen with the check pipeline; Open tube type resistance furnace and carry out heat treated, open hydrogenchloride gas cylinder reducing valve simultaneously, continue to feed dry hydrogen chloride in stove, air flow maintains 0.5~1 liter/minute.In roasting processed process, the maturing temperature that progressively raises is incubated earlier roasting 0.5 hour respectively under 100 ℃, 150 ℃, 200 ℃, and the furnace temperature to 250 that raises again ℃ was carried out the roasting processed 5 hours, made LaCl 37H 2O progressively sloughs contained crystal water, and water vapor continue to be discharged along with hci gas flow, gradually condensation and splash into the glass surge flask; Adopt diluted sodium hydroxide solution absorbing hydrogen chloride tail gas.The roasting processed comparatively fast is cooled near room temperature furnace temperature after finishing, and feeds high pure nitrogen with hydrogen chloride gas in the pipe blow-through, takes out treated powder rapidly, is sealed preservation.
(2) with 5000g LaCl 37H 2O contains into the boat-shaped quartz glass crucibles, is positioned over the middle part of quartz glass tube in the tube type resistance furnace; Connect whole breather line system, feed the resistance to air loss of high pure nitrogen with the check pipeline; Open tube type resistance furnace and carry out heat treated, continue simultaneously to feed dry hydrogen chloride in stove, air flow maintains 1.5~3 liters/minute.Be incubated earlier roasting 0.5 hour under 100 ℃, 150 ℃, 200 ℃ respectively, the furnace temperature to 230 that raises again ℃ was carried out the roasting processed 8 hours; Adopt diluted sodium hydroxide solution absorbing hydrogen chloride tail gas.The roasting processed comparatively fast is cooled near room temperature furnace temperature after finishing, and feeds high pure nitrogen with hydrogen chloride gas in the pipe blow-through, takes out treated powder rapidly, is sealed preservation.

Claims (4)

1、无水氯化镧的氯化焙烧脱水法制备工艺,其特征在于:以LaCl3·7H2O为初始原料,采用干燥氯化氢保护下的焙烧脱水处理,在充分有效地抑制水解反应的条件下,使LaCl3·7H2O逐步脱去所含结晶水,以制备较高纯度的无水氯化镧试剂。1. The preparation process of anhydrous lanthanum chloride by chlorination roasting dehydration method, which is characterized in that: using LaCl 3 7H 2 O as the initial raw material, adopting roasting dehydration treatment under the protection of dry hydrogen chloride, under the condition of fully and effectively inhibiting the hydrolysis reaction Under the following conditions, the LaCl 3 ·7H 2 O is gradually removed from the contained crystal water to prepare anhydrous lanthanum chloride reagent of higher purity. 2、按权利要求1所述的无水氯化镧制备工艺,其特征在于:焙烧温度须控制于200~300℃,以避免发生明显水解反应。2. The process for preparing anhydrous lanthanum chloride according to claim 1, characterized in that the roasting temperature must be controlled at 200-300°C to avoid obvious hydrolysis reaction. 3、按权利要求1或2所述的无水氯化镧制备工艺,其特征在于:须持续通入足量干燥氯化氢气体,以完全抑制发生水解反应。3. The process for preparing anhydrous lanthanum chloride according to claim 1 or 2, characterized in that: a sufficient amount of dry hydrogen chloride gas must be fed continuously to completely suppress the hydrolysis reaction. 4、按权利要求1或2或3所述的无水氯化镧制备工艺,其特征在于:经过5~10小时焙烧处理,以脱去LaCl3·7H2O所含全部水分。4. The process for preparing anhydrous lanthanum chloride according to claim 1, 2 or 3, characterized in that it is roasted for 5-10 hours to remove all the water contained in LaCl 3 ·7H 2 O.
CN 200610067759 2006-03-14 2006-03-14 Preparation technique of anhydrous lanthanum chloride by chlorination baking dehydration method Pending CN101037216A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN 200610067759 CN101037216A (en) 2006-03-14 2006-03-14 Preparation technique of anhydrous lanthanum chloride by chlorination baking dehydration method

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN 200610067759 CN101037216A (en) 2006-03-14 2006-03-14 Preparation technique of anhydrous lanthanum chloride by chlorination baking dehydration method

Publications (1)

Publication Number Publication Date
CN101037216A true CN101037216A (en) 2007-09-19

Family

ID=38888424

Family Applications (1)

Application Number Title Priority Date Filing Date
CN 200610067759 Pending CN101037216A (en) 2006-03-14 2006-03-14 Preparation technique of anhydrous lanthanum chloride by chlorination baking dehydration method

Country Status (1)

Country Link
CN (1) CN101037216A (en)

Cited By (15)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
RU2422365C1 (en) * 2009-11-19 2011-06-27 Гоу Впо "Сибирский Государственный Индустриальный Университет" Apparatus for producing anhydrous lanthanide trichlorides
CN102781894A (en) * 2010-03-04 2012-11-14 陶氏环球技术有限责任公司 Process for producing methyl chloride and sulfur dioxide
RU2471710C1 (en) * 2011-05-31 2013-01-10 Учреждение Российской Академии Наук Институт Нефтехимии И Катализа Ран Method of obtaining compounds of divalent lanthanides
CN103691337A (en) * 2013-12-12 2014-04-02 宁夏东方钽业股份有限公司 Preparation method of anhydrous lanthanum chloride and halogen salt mixture
CN104973617A (en) * 2015-07-01 2015-10-14 乐山沃耐稀电子材料有限公司 Preparation method of anhydrous lanthanum chloride
CN106915763A (en) * 2017-05-02 2017-07-04 乐山沃耐稀电子材料有限公司 A kind of high-purity anhydrous lanthanum chloride preparation technology
CN107487778A (en) * 2016-06-13 2017-12-19 有研稀土新材料股份有限公司 High-pure anhydrous rare earth halide and preparation method thereof
CN107604385A (en) * 2017-09-12 2018-01-19 中国科学院青海盐湖研究所 Magnesium-rare earth alloy is electrolysed the preparation method of raw material
CN112607761A (en) * 2020-12-28 2021-04-06 包头市明芯科技有限公司 Preparation method of high-purity anhydrous rare earth chloride
CN113800551A (en) * 2021-10-27 2021-12-17 福建省长汀金龙稀土有限公司 Method for preparing rare earth oxide powder by utilizing steam roasting of rare earth chloride
CN113830818A (en) * 2021-10-11 2021-12-24 天津包钢稀土研究院有限责任公司 Preparation method of anhydrous rare earth halide
CN114634198A (en) * 2022-03-31 2022-06-17 山东金能环保科技有限公司 Preparation method of high-purity anhydrous lanthanum chloride
CN114772627A (en) * 2022-03-30 2022-07-22 蜂巢能源科技(无锡)有限公司 Dehydration purification method and application of solid electrolyte
CN115520891A (en) * 2022-08-26 2022-12-27 内蒙古医科大学 Preparation method and application of potential medicament lanthanum chloride for effectively improving vascular calcification
CN116332220A (en) * 2023-05-29 2023-06-27 研峰科技(北京)有限公司 Synthesis method of lanthanum (III) chloride bis (lithium chloride)

Cited By (20)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
RU2422365C1 (en) * 2009-11-19 2011-06-27 Гоу Впо "Сибирский Государственный Индустриальный Университет" Apparatus for producing anhydrous lanthanide trichlorides
CN102781894A (en) * 2010-03-04 2012-11-14 陶氏环球技术有限责任公司 Process for producing methyl chloride and sulfur dioxide
CN102781894B (en) * 2010-03-04 2014-11-05 陶氏环球技术有限责任公司 Process for producing methyl chloride and sulfur dioxide
RU2471710C1 (en) * 2011-05-31 2013-01-10 Учреждение Российской Академии Наук Институт Нефтехимии И Катализа Ран Method of obtaining compounds of divalent lanthanides
CN103691337A (en) * 2013-12-12 2014-04-02 宁夏东方钽业股份有限公司 Preparation method of anhydrous lanthanum chloride and halogen salt mixture
CN104973617A (en) * 2015-07-01 2015-10-14 乐山沃耐稀电子材料有限公司 Preparation method of anhydrous lanthanum chloride
CN107487778A (en) * 2016-06-13 2017-12-19 有研稀土新材料股份有限公司 High-pure anhydrous rare earth halide and preparation method thereof
CN107487778B (en) * 2016-06-13 2019-12-31 有研稀土新材料股份有限公司 High-purity anhydrous rare earth halide and preparation method thereof
CN106915763A (en) * 2017-05-02 2017-07-04 乐山沃耐稀电子材料有限公司 A kind of high-purity anhydrous lanthanum chloride preparation technology
CN107604385A (en) * 2017-09-12 2018-01-19 中国科学院青海盐湖研究所 Magnesium-rare earth alloy is electrolysed the preparation method of raw material
CN112607761A (en) * 2020-12-28 2021-04-06 包头市明芯科技有限公司 Preparation method of high-purity anhydrous rare earth chloride
CN112607761B (en) * 2020-12-28 2022-04-08 包头市明芯科技有限公司 Preparation method of high-purity anhydrous rare earth chloride
CN113830818A (en) * 2021-10-11 2021-12-24 天津包钢稀土研究院有限责任公司 Preparation method of anhydrous rare earth halide
CN113800551A (en) * 2021-10-27 2021-12-17 福建省长汀金龙稀土有限公司 Method for preparing rare earth oxide powder by utilizing steam roasting of rare earth chloride
CN114772627A (en) * 2022-03-30 2022-07-22 蜂巢能源科技(无锡)有限公司 Dehydration purification method and application of solid electrolyte
CN114772627B (en) * 2022-03-30 2024-02-13 蜂巢能源科技(无锡)有限公司 Dehydration purification method and application of solid electrolyte
CN114634198A (en) * 2022-03-31 2022-06-17 山东金能环保科技有限公司 Preparation method of high-purity anhydrous lanthanum chloride
CN115520891A (en) * 2022-08-26 2022-12-27 内蒙古医科大学 Preparation method and application of potential medicament lanthanum chloride for effectively improving vascular calcification
CN116332220A (en) * 2023-05-29 2023-06-27 研峰科技(北京)有限公司 Synthesis method of lanthanum (III) chloride bis (lithium chloride)
CN116332220B (en) * 2023-05-29 2023-08-11 研峰科技(北京)有限公司 Synthesis method of lanthanum (III) chloride bis (lithium chloride)

Similar Documents

Publication Publication Date Title
CN101037216A (en) Preparation technique of anhydrous lanthanum chloride by chlorination baking dehydration method
CN102502739A (en) Method for producing high-purity alpha-aluminum oxide
CN104003443B (en) A kind of method adding JZPD capsule ammonium meta-vanadate
CN103184354A (en) Preparation method of high-purity arsenic
CN110015671A (en) A kind of preparation method of high-purity magnesium oxide
CN103241754A (en) Production method of high-purity aluminum oxide
CN111675195A (en) Energy-saving environment-friendly process flow for synthesizing hydrochloric acid
CN108328642A (en) A method of non-evaporating hair prepares basic zinc carbonate from zinc ammonia solution
CN105347703B (en) A kind of decomposition method of calcium carbonate and magnesium carbonate ore deposit
WO2018040998A1 (en) Method for preparing new ultra-pure spherical alumina powder
CN114735691A (en) Process for purifying high-purity carbon powder
CN104495884B (en) basic magnesium carbonate and preparation method thereof
Shayanfar et al. Thermodynamic modeling and experimental studies of Bayerite precipitation from aluminate solution: temperature and pH effect
CN105540648A (en) Preparation method of stannic oxide mesoporous spheres
CN106220534B (en) A kind of preparation facilities and preparation method of biruea
CN106986359B (en) The device and method of chlorinity in product magnesia is reduced in a kind of magnesium hydroxide calcination process
CN107758731A (en) A kind of method and apparatus for preparing titanium trichloride powder
CN102060279B (en) Device and method for synthesizing zinc germanium phosphide polycrystal
CN117228708A (en) Method for promoting stannous chloride to crystallize rapidly
CN103803622A (en) Method using aluminum chloride hexahydrate dehydration to prepare anhydrous aluminum chloride
CN104495885B (en) A kind of method utilizing magnesium halogen crystalline substance high purity magnesium chloride
CN113044862B (en) A method for dehydrating different ammonium carnallite materials by utilizing the synergistic coupling effect between them
CN105329920A (en) Method for joint production of potassium sulphate and calcium chloride dihydrate
CN109517006B (en) Method for continuously producing 3-octanoyl thiopropyl triethoxysilane by tower-type organic method
CN113375432A (en) Anhydrous rare earth halide purification dewatering equipment

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C02 Deemed withdrawal of patent application after publication (patent law 2001)
WD01 Invention patent application deemed withdrawn after publication

Open date: 20070919