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Preformed catalytic system comprising a rare-earth metallocene

一种催化体系、稀土金属的技术，应用在制备所述催化体系领域，能够解决降低生产装置生产量、运行复杂化等问题

Active Publication Date: 2019-04-02
MICHELIN & CO (CIE GEN DES ESTAB MICHELIN)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The regulating and stabilizing phases have the effect of reducing the throughput of the production plant and complicating its operation

Method used

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  • Preformed catalytic system comprising a rare-earth metallocene
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  • Preformed catalytic system comprising a rare-earth metallocene

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preparation example Construction

[0085] b) Polymer preparation:

[0086] The polymer samples were not specially treated prior to analysis. It was simply dissolved in tetrahydrofuran + 0.1% by volume distilled water at a concentration of about 1 g / l. The solution was then filtered through a filter with a porosity of 0.45 μm before injection.

[0087] c) SEC analysis:

[0088] The apparatus used was a Waters Alliance chromatograph. The elution solvent was tetrahydrofuran, the flow rate was 0.7 ml / min, the system temperature was 35° C. and the analysis time was 90 minutes. A set of four Waters columns in series having the trade designations Styragel HMW7, Styragel HMW6E and two Styragel HT6E was used.

[0089] The volume of the injected polymer sample solution was 100 µl. The detector was a Waters 2410 differential refractor and the software to use the chromatographic data was a Waters Empower system.

[0090] Calculated average molar masses are relative to a calibration curve generated from commercial...

Embodiment 1 to 11

[0092] The catalytic systems C1 to C11 according to the invention were prepared according to the following procedure.

[0093] At the levels shown in Table I, the cocatalyst butyloctylmagnesium (BOMAG) followed by the metallocene [Me 2 Si(Flu) 2 Nd(μ-BH 4 ) 2Li(THF)] was added to a reactor containing the hydrocarbon solvent methylcyclohexane (MCH) or toluene (Tol). The activation time was 10 minutes and the reaction temperature was 20° C. (step a)). Subsequently, the preformed monomers, which are ethylene (Eth), a mixture of ethylene and 1,3-butadiene (Eth / Bde), or a mixture of ethylene and isoprene (Eth / Iso)) into the reactor, the mole fraction of ethylene in the mixture of ethylene and 1,3 butadiene or ethylene and isoprene is 0.8. The preforming reactions were carried out at the temperatures indicated in Table I for the time periods also indicated in Table I. In Example 4, at the end of step b), the reactor was degassed and flushed with nitrogen to remove unconverted...

Embodiment 12 to 14

[0095] The catalytic system CE1-1 not in accordance with the present invention was prepared according to the method disclosed in the patent application WO 2007054224 and described as follows:

[0096] At the levels shown in Table II, the cocatalyst butyloctylmagnesium (BOMAG) followed by the metallocene [Me 2 Si(Flu) 2 Nd(μ-BH 4 ) 2 Li(THF)] was added to the reactor containing toluene (Tol). The activation time is 10 minutes, and the reaction temperature is 20°C. Its preparation conditions are shown in Table II.

[0097] Catalytic system CE1-2 not in accordance with the invention was prepared in a similar manner to catalytic system CE1-1, except that the solvent was methylcyclohexane.

[0098] Catalyst systems CE1-3 not in accordance with the invention were prepared according to the following procedure:

[0099] At the levels shown in Table II, the cocatalyst butyloctylmagnesium (BOMAG) followed by the metallocene [Me 2 Si(Flu) 2 Nd(μ-BH 4 ) 2 Li(THF)] was added to a...

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Abstract

The present invention relates to a catalytic system made of at least one preforming monomer which is ethylene or a mixture of ethylene and a conjugated diene, a metallocene of formula{P(Cp1)(Cp2)Y} orCp3Cp4Y, an organometallic compound as a co-catalyst, Y designating a group comprising a rare-earth metal atom, the groups Cp1, Cp2, Cp3 and Cp4, identical or different, being selected from the groupmade up of the fluorenyl groups, the cyclopentadienyl groups and the indenyl groups, the groups being optionally substituted, P being a group bridging the two groups Cp1 and Cp2, and comprising a silicon or carbon atom. Such a catalytic system has improved stability of the catalytic activity over time, in particular during storage.

Description

technical field [0001] The present invention relates to preformed catalytic systems based on rare earth metallocenes which can be used in particular for the polymerization of monomers such as conjugated dienes, ethylene, alpha-monoolefins and mixtures thereof. The invention also relates to a process for the preparation of said catalytic system and its use in polymer synthesis. Background technique [0002] Catalytic systems based on rare earth metallocenes are known: they are described, for example, in patent applications EP 1 092 731 , WO 2004035639 and WO 2007054224 in the name of the applicant company for monomers such as conjugated dienes, ethylene and Polymerization of alpha-monoolefins. They are the reaction products of lanthanide metallocenes and cocatalysts in hydrocarbon solvents. The catalytic systems thus formed have the disadvantage that their catalytic activity decreases on storage. In order to guarantee the technical parameters of the polymers to be synthesi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F17/00C07F5/00C08F4/54C08F10/02
CPCC07F17/00C07F5/00C08F236/06C08F210/02C08F4/52C07F3/02C08F110/02C08F210/18C08F236/08C08F2420/01
Inventor V·拉法奎尔J·蒂耶
Owner MICHELIN & CO (CIE GEN DES ESTAB MICHELIN)
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