SU1184814A1 - Method of producing thiotetrachlorides of tungsten and molybdenum - Google Patents

Method of producing thiotetrachlorides of tungsten and molybdenum Download PDF

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Publication number
SU1184814A1
SU1184814A1 SU843768415A SU3768415A SU1184814A1 SU 1184814 A1 SU1184814 A1 SU 1184814A1 SU 843768415 A SU843768415 A SU 843768415A SU 3768415 A SU3768415 A SU 3768415A SU 1184814 A1 SU1184814 A1 SU 1184814A1
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USSR - Soviet Union
Prior art keywords
tungsten
thiotetrachlorides
producing
molybdenum
solvent
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SU843768415A
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Russian (ru)
Inventor
Владимир Ефимович Федоров
Владимир Петрович Федин
Ольга Анатольевна Кузьмина
Петр Петрович Семянников
Original Assignee
Новосибирский государственный университет им.Ленинского комсомола
Институт Неорганической Химии Со Ан Ссср
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Priority to SU843768415A priority Critical patent/SU1184814A1/en
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Publication of SU1184814A1 publication Critical patent/SU1184814A1/en

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  • Inorganic Compounds Of Heavy Metals (AREA)

Description

00 1 Изобретение относитс  к неорганической химии, а именно к синтезу халькогенгалогенидов вольфрама и молибдена, которые могут найти прим нение в качестве катодных материалов дл  химических источников тока, в препаративной химии, как исходный материал дл  различных синтезов. Цель изобретени  - повьшение чис тоты продуктов. П р и м е р 1. К 5,20 г W(CO)g в 30 мл абсолютного гексана добавл ют 10 мл SCl, реакционную смесь нагревают при 64 С до прекращени  в делени  газа. Выпавший осадок отфильтровали и высушили в при при . Все операции проведены за 3 ч. Получено 5,05 г целевого продукта , что составл ет 96% от теор. Найдено,%: W5,61; 5 8,85; 01 39,5. W 51,39; S 8,97; Вычислено,%; С1 39,64. 2. К 5,0 г Mo(COJt в Пример 30 мл гексана добавл ют 10 мл SCl По окончании выделени  газов и выпа 42 дении осадка реакционную смесь отфильтровывают , промывают хлороформом и осадок высушивают в вакууме при 150С. Синтез идет при комнатной температуре от нескольких минут до 1 ч. Побочные продукты синтеза выдел ютс  при этом из реакционной смеси в газообразном виде, сера раствор етс  в избытке хлоридов, а целевой продукт (осадок ) извлекают фильтрацией . Получено 4,2 г целевого продукта , что составл ет 95% от теор. Найдено,%: Мо 40,88; S 13,65; С1 45,47. MoSCIJ. Вычислено,%: Мо 40,94-, S 13,68; С1 45,38. П р и м е р 3. При соблюдении параметров примера 2 в качестве, растворител  берут ССЦ. Получено 4,12 г (98%) MoSCl}. П р и м е р 4. При соблюдении условий примера 2 в качестве растворител  берут CHClj. Получено 4,2 г (95% ) МоЗСЦ .00 1 The invention relates to inorganic chemistry, namely to the synthesis of tungsten and molybdenum chalcogen halides, which can be used as cathode materials for chemical current sources, in preparative chemistry, as a starting material for various syntheses. The purpose of the invention is to increase the purity of the products. EXAMPLE 1. To 5.20 g of W (CO) g in 10 ml of absolute hexane, 10 ml of SCl is added, the reaction mixture is heated at 64 ° C until it stops in gas separation. The precipitate was filtered and dried at at. All operations were carried out in 3 hours. 5.05 g of the expected product was obtained, which is 96% of the theory. Found,%: W5.61; 5 8.85; 01 39.5. W 51.39; S 8.97; Calculated,%; C1 39.64. 2. To 5.0 g of Mo (COJt in Example 30 ml of hexane is added 10 ml of SCl. After the evolution of gases and precipitation of precipitate has formed, the reaction mixture is filtered, washed with chloroform and the precipitate is dried in vacuum at 150 ° C. The synthesis proceeds at room temperature from a few minutes to 1 hour. The synthesis byproducts are separated from the reaction mixture in gaseous form, sulfur is dissolved in an excess of chlorides, and the target product (precipitate) is removed by filtration. 4.2 g of the expected product is obtained, which accounts for 95% of Found,%: Mo 40.88; S 13.65; C1 45.47. MoSCIJ. Calculated,%: Mo 40.94-, S 13.68; C1 45.38. EXAMPLE 3. If the parameters of Example 2 are observed, the SSC is taken as the solvent, 4.12 g (98%) of MoSCl} is obtained. measure 4. If the conditions of example 2 are observed, take CHClj as the solvent. 4.2 g (95%) MOFC were obtained.

Claims (2)

(5^) 1.СПОСОБ ПОЛУЧЕНИЯ ТИОТЕТРАХЛОРИДОВ ВОЛЬФРАМА И МОЛИБДЕНА взаимодействием металлсодержащего соединения с хлоридом серы, отличающийся тем, что, с .целью повышения чистоты продуктов, в качестве исходного металлсодержаще· го соединения используют гексакарбонил вольфрама или молибдена и процесс ведут в среде органического растворителя.(5 ^) 1. METHOD FOR PRODUCING TUNGSTEN AND MOLYBDENE THIOTETRACHLORIDES by reacting a metal-containing compound with sulfur chloride, characterized in that, in order to increase the purity of the products, tungsten or molybdenum hexacarbonyl in an organic medium is used and the solvent is used . 2. Способ поп.1,отличающ и й с я тем, что, с целью повышения выхода тиотетрахлорида вольфрама, в качестве хлорида серы иС-~ пользуют дихлоромоносульфан, а в качестве растворителя - гексан при температуре его кипения.2. The method of pop. 1, characterized in that, in order to increase the yield of tungsten thiotetrachloride, dichloromonosulfan is used as sulfur chloride and C- ~, and hexane is used as a solvent at its boiling point.
SU843768415A 1984-05-30 1984-05-30 Method of producing thiotetrachlorides of tungsten and molybdenum SU1184814A1 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
SU843768415A SU1184814A1 (en) 1984-05-30 1984-05-30 Method of producing thiotetrachlorides of tungsten and molybdenum

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
SU843768415A SU1184814A1 (en) 1984-05-30 1984-05-30 Method of producing thiotetrachlorides of tungsten and molybdenum

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SU1184814A1 true SU1184814A1 (en) 1985-10-15

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Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
.D. Britnell et a1.Preparation of Halide Suj phides and Selenides of Mqlibdenium and Tungsten y.c.s. Dalton Trans,1974, p..p.2191-2194. Авторское свидетельство СССР № 220974, кл. С 01 G 41/00, 1967. Фортунатов Н.С., Тимощенко А. И. О новом тиохлориде вольфрама.Украинский химический журнал,1969, т.35, вып.11, с.1207-1209. *

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