WO2003095465A1 - Procede d'obtention d'halogenures de metallocenes - Google Patents

Procede d'obtention d'halogenures de metallocenes Download PDF

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Publication number
WO2003095465A1
WO2003095465A1 PCT/RU2003/000212 RU0300212W WO03095465A1 WO 2003095465 A1 WO2003095465 A1 WO 2003095465A1 RU 0300212 W RU0300212 W RU 0300212W WO 03095465 A1 WO03095465 A1 WO 03095465A1
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WO
WIPO (PCT)
Prior art keywords
target product
amine
fact
hours
egο
Prior art date
Application number
PCT/RU2003/000212
Other languages
English (en)
Russian (ru)
Inventor
Alexsandr Sergeevich Smirnov
Alexsandr Alekseevich Aladiin
Aleksei Nikolaevich Tatarnikov
Nadezda Jurievna Kabarova
Original Assignee
Obshestvo S Ogranichennoi Otvetstvennostju Synor
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 Obshestvo S Ogranichennoi Otvetstvennostju Synor filed Critical Obshestvo S Ogranichennoi Otvetstvennostju Synor
Priority to AU2003241976A priority Critical patent/AU2003241976A1/en
Publication of WO2003095465A1 publication Critical patent/WO2003095465A1/fr

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
    • C07F17/00—Metallocenes

Definitions

  • Metal halides are used as a catalyst for industrial use and polypropylene.
  • the diethylamine used in this system is a one-time and a consumer, and there is no excess in it, and there is no loss of life
  • the resulting mixture after the indicated interaction, is washed with diluted salted acid, after which the target product is isolated by extraction.
  • the dedicated product is vacuum-dried with the following clean installation (patent U.S. 23071605, claimed 02.15.1955).
  • the yield of the product is 35-37%. Waste of the system is a large part of the process and labor, including the long-term operation of the extraction, which is not necessary for the separation of the costs of May, the stage of removal of the solvent under vacuum.
  • the objective of the invention is to simplify and reduce the cost.
  • the method provides for the receipt of the target product with a yield of 55-60% for halide and residential prices and 80-90% for utility costs.
  • a customer can buy products with the indicated contents of basic materials and clean them, which is necessary for the commercialization.
  • EXAMPLE 1 In a central flask equipped with a refrigeration and stirrer, in the atmosphere, pour in 0.9 ml (100 ml) of flour, which gives 2.3 ml (155 ml), d) cycle-pentadiene, the mixture is heated up to 60 ° ⁇ - the temperature of the accumulation of coolant, and the resulting mass is maintained for 7 hours. They receive a suspension of dark-colored colors, in addition to adding a methane for a complete expansion of the amine of the salt acid. Then the target product is isolated by filtration and dried on the air for 10-12 hours. Crystals bis (cyclopentadienyl) titanium oxide ⁇ _ % .
  • the output of the product is 85%, the content of the main material is 90%.
  • the received product is in the process of transferring from the housing. After the installation is complete, the content of the basic material, according to the method, is 98%. Melting point 288 ° ⁇ . Elemental analysis data are consistent with the theory.
  • EXAMPLE 2 Implementation of the method under conditions of an industrial application.
  • ⁇ The cooled mass is added 10 l of methanol for the complete dissolution of the amine of the salt acid. Then 6
  • the target product is isolated by filtering and dried in the air.
  • P ⁇ luchayu ⁇ is ⁇ ally bis (tsi ⁇ l ⁇ en ⁇ adienil) ⁇ i ⁇ andi ⁇ l ⁇ ida - - (C 5 ⁇ 5) 2 ⁇ / -.
  • EXAMPLE 3 The conditions of the test experience in Example 1, only in the quality of metal halide, 0.9 mol (209 g) of cytotoxide and process are conducted. As described in Example 1. Receive bis (cyclopentadienyl) crystals ⁇ lorida - ( ⁇ ⁇ ⁇ ⁇ ) ⁇ ⁇ ⁇
  • the output of the product is 53%, the content of the main material is 88%, after the removal of the product - 99%
  • Example 4 The conditions of the test in Example 3, only in the quality of metal halide, are not affected by hafnium. Crystals bis (cyclopentadienyl) hafnium dihydride - (C ⁇ ⁇ ⁇ ) ⁇ ⁇ * s ⁇
  • the yield of the product is 53%, the content of the main material, according to the method of YaS, is 90%, after the process of industrialization - 98%.
  • Example 5 The conditions of the case in Example 2, only methyl cyclopentadiene are used in place of cyclic pentadiene. Titanium bis (methyl-cyclopentadienyl) titanium is “The yield of the product is 80%, the content of the main material is 90, after the installation, it is 98.
  • EXAMPLE 6 Conditions of the test experience in Example 2, since instead of cyclopentadiene, pentamethylcyclopentadiene is absent. It is produced di ⁇ lobbis (pentamethylcyclopentadienyl) titanium - (Less than 5 C 5 ) ⁇ ⁇ . The yield is 85, the composition of the main substance is 7 stays at the level of 90%, after pre-installation - 98%
  • Example 7 The conditions of the test in Example 1, only a titanium oxide, but a titanium oxide, are treated together with titanium. Receive crystals of bis (cyclopentadienyl) titanium dibamide - The yield of the product is 85%, the content of the main material is at the level of 90%, after the installation of the house - 99%.
  • halides of metals are commensurate with the invention, saves the use of cheaper products, which, in general, reduces the cost of production.
  • the method can be used under conditions of industrial use, t. ⁇ . It is quite simple and not long in use.
  • Metallic halides are used as a catalyst for industrial and industrial use (polyethylene, polyethylene, polyethylene, and benzene are obtained).

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)

Abstract

L'invention a trait à un procédé d'obtention d'halogénures de métallocènes représentés par la formule générale Cp2MX2 (1), dans laquelle Cp représente une composition cyclopentadiène, M représente un métal du groupe IVB (Zr, Hf, Ti), X représente un halogène. Ledit procédé consiste : à synthétiser par interréaction un halogénure d'un métal correspondant avec un système cyclopentadiène et de la diéthylamine, les réactifs étant présents dans un rapport molaire égal à 1: (2-2, 5): 2 respectivement, dans un milieu chloroforme à la température d'ébullition de ce dernier, de préférence dans une atmosphère de gaz inerte, ladite synthèse s'effectuant en 2 à 10 heures ; à séparer le produit cible du chlorure d'amine par dissolution de ce dernier dans un alcool aliphatique ; à extraire ensuite le produit cible par filtrage, et à le sécher. Ledit procédé permet d'obtenir un produit cible ayant un rendement de 55-60 % d'halogénures d'hafnocène et de zirconocène, et de 80-90 % d'halogénures de titanocène, avec une teneur en composé principal s'élevant à 90 %. Afin d'obtenir des produits présentant une teneur élevée en composé principal, atteignant les 98-99 %, on purifie le produit cible, après séchage, par recristallisation.
PCT/RU2003/000212 2002-05-13 2003-05-12 Procede d'obtention d'halogenures de metallocenes WO2003095465A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AU2003241976A AU2003241976A1 (en) 2002-05-13 2003-05-12 Method for producing metallocene halides

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
RU2002112538 2002-05-13
RU2002112538/04A RU2214415C1 (ru) 2002-05-13 2002-05-13 Способ получения галогенидов металлоценов (варианты)

Publications (1)

Publication Number Publication Date
WO2003095465A1 true WO2003095465A1 (fr) 2003-11-20

Family

ID=29417891

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/RU2003/000212 WO2003095465A1 (fr) 2002-05-13 2003-05-12 Procede d'obtention d'halogenures de metallocenes

Country Status (3)

Country Link
AU (1) AU2003241976A1 (fr)
RU (1) RU2214415C1 (fr)
WO (1) WO2003095465A1 (fr)

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103725901B (zh) * 2013-12-12 2015-10-28 上海哈峰新材料科技有限公司 氧化锆/氧化铪混合物的火法分离方法

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3071605A (en) * 1955-02-15 1963-01-01 Union Carbide Corp Process for producing cyclopentadienyl-type metallic compounds
US5708150A (en) * 1994-12-22 1998-01-13 Witco Gmbh Process for preparing transition metal complexes containing disubstituted cyclopentadienyl ligands
RU2156253C2 (ru) * 1994-01-19 2000-09-20 Бп Кемикэлс Лимитед Каталитическая композиция, металлоценовый комплекс и способ полимеризации олефинов

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3071605A (en) * 1955-02-15 1963-01-01 Union Carbide Corp Process for producing cyclopentadienyl-type metallic compounds
RU2156253C2 (ru) * 1994-01-19 2000-09-20 Бп Кемикэлс Лимитед Каталитическая композиция, металлоценовый комплекс и способ полимеризации олефинов
US5708150A (en) * 1994-12-22 1998-01-13 Witco Gmbh Process for preparing transition metal complexes containing disubstituted cyclopentadienyl ligands

Also Published As

Publication number Publication date
RU2214415C1 (ru) 2003-10-20
AU2003241976A1 (en) 2003-11-11

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