A kind of synthetic method of metallocene catalyst

Abstract

The invention provides a method for synthesizing a metallocene catalyst (Ind)2ZrCl2. The method comprises the following steps that lithium salt is prepared from indene in a mixed solvent of ethers and arenes at room temperature, trimethylchlorosilane or trimethyltin chloride are added to the lithium salt and a 1-substituted indenyl compound is generated; the substituted indenyl compound reacts with zirconium tetrachloride at room temperature to synthesize the metallocene catalyst, the product is simply washed with a mixed solvent of alcohols and ethers and simply filtered, and then the (Ind)2ZrCl2 can be synthesized with a high yield. According to the method, a low temperature reaction is omitted, the operation conditions are mild, the high-purity metallocene compound can be obtained by means of the simple washing and filtering methods, the complicated purification steps, such as extraction and sublimation, are omitted, and the method is beneficial to industrial production.

Description

technical field [0001] The present invention relates to the field of synthesis of organometallic catalysts, in particular to the main catalyst metallocene catalyst (Ind) for olefin polymerization 2 ZrCl 2 synthetic method. Background technique [0002] Metallocene catalysts are composed of transition metal zirconium, titanium or hafnium and one or more cyclopentadienyl or substituted cyclopentadienyl, or with a multi-ring structure containing cyclopentadiene ring [such as indenyl (Ind) , fluorenyl (Flu)] and other atoms or groups formed organometallic complexes and co-catalysts (in some cases, a carrier is also required). Among them, an organometallic compound having a cyclopentadienyl structure directly bonded to a transition metal is called a "metallocene compound". [0003] Compared with traditional Ziegler-Natta catalysts, metallocene catalysts have the following characteristics: First, metallocene catalysts have a single catalytic active center, which is the main dif...

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Problems solved by technology

[0007] The above synthesis (Ind) 2 ZrCl 2 There are obvious shortcomings in the routes: first, most of the reactions need to be carried out at ultra-low temperature (-78°C), which consumes a lot of energy, greatly increases the cost and difficulty of catalyst synthesis, and hinders its industrial scale-up. production; secondly in the above-mentioned synthetic process, the purification of the catalyst all needs to adopt methods such as distillation, filtration, extraction, washing and sublimation, and the operation process is loaded down with trivial details and inefficiency; Finally, the yield of above-mentioned synthetic method is mostly low, about 50%

Although Balboni Davide et al. obtained a high yield of 96% in the synthesis process, the cost is to use twice as much methyllithium ether solution, and the nature of methyllithium ether solution is very active, which brings more safety to its use. high requirements

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