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Catalyst system for ethylene selective oligomerization, preparation method and ethylene oligomerization reaction method
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A catalyst and selectivity technology, applied in the field of catalysis, can solve the problems of low total selectivity of 1-hexene and 1-octene, large amount of activator, etc., and achieve the effects of low cost, long catalyst life and simple synthesis
Active Publication Date: 2020-11-06
TIANJIN UNIV OF SCI & TECH
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[0006] In view of this, the present invention aims to propose a catalyst system for ethylene selective oligomerization, to solve the technology that the total selectivity of 1-hexene and 1-octene is not high and the amount of activator is large in the ethylene oligomerization reaction question
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[0108] In one embodiment of the present invention, the preparation method of catalyst system comprises the following steps:
[0109] Components a, b, and c are pre-mixed or directly added to the reaction system for in-situ synthesis. That is to say, the catalyst is prepared by pre-mixing ligand a, transition metal compound b, and activator c connected by a linking group containing heteroatoms; it is also possible to mix the ligands connected by chain groups containing heteroatoms a, the transition metal compound b, and the activator c are directly added to the reaction system for in-situ synthesis;
[0110] The reaction mode of ligand a, transition metal compound b and activator c connected by a linking group containing heteroatoms in general formula I can be reacted by liquid phase, such as reacting under the action of a solvent, and the optional solvent Such as toluene, benzene and its derivatives, etc.; also through solid-state reaction; or through in-situ reaction in the ...
Embodiment 1
[0119] 1. Preparation of ligands:
[0120] When A is -CH 2 (CH 3 ) 2 SiCH 2 -, E is a sulfur atom, R 1 Is isopropyl, R 2 is phenyl, R 3 is cyclopentyl, and the ligand is N-((cyclopentylmercaptomethyl)dimethylsilyl)-1,1-diisopropyl-N-phenylphosphineamine (C 21 h 38 NPSSi)
[0122] in the N 2 Add dehydrated THF (200ml) and aniline (9.31g, 0.1mol) into a fully replaced stirred 500ml reactor, stir well and cool to -78°C with liquid nitrogen. Use a 100ml syringe to extract n-butyllithiumhexane solution (41.6ml, 2.4mol / L), slowly add it dropwise to the above solution while stirring, keep stirring at -78°C for 1h, then rise to room temperature and continue stirring for 1 hour, then vacuum pump The solvent was removed, n-hexane (100ml) was added, stirred and dispersed, and then filtered. The obtained filtrate was vacuum-extracted at room temperature to obtain 9.97g (0.098mol, 97.8%) of the product.
[0123] (2) prepare 1,1-diiso...
Embodiment 2
[0139] With embodiment 1. The difference is that R 2 For 2,6-diisopropylphenyl. 135.7 g of oligomerization product was obtained, and the catalyst activity was 8.22×10 6 g oligomer / mol Cr·h. The distribution of the oligomerization products is shown in Table 1.
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Abstract
The invention provides a catalyst system for selective oligomerization of ethylene, which belongs to the technical field of catalysis. The catalyst system includes three components: ligand a; transition metal compound b, which is a metal compound of groups IVB to VIII; wherein ligand a contains at least one group represented by the general formula I, the general formula I is as follows: The connecting group A of the general formula I has a main chain including an alkyl group, an alkenyl group or an aryl group and a connecting group composed of a heteroatom, wherein the heteroatom is one of silicon, tin, boron, phosphorus and nitrogen; Group E is the sixth main group elementoxygen or sulfur; R 1 ,R 2 ,R 3 are the substituent groups on the phosphorus atom, nitrogen atom and group E respectively, R 1 ,R 2 ,R 3 Same or different. The catalyst system of the invention has high activity, high selectivity of target products 1-hexene and 1-octene, and C in the product 6 ~C 8 The mass percentage of linear α-olefins is >90%, and the catalyst is simple to synthesize, low in cost and long in life.
Description
technical field [0001] The invention belongs to the technical field of catalysis, and relates to a catalyst system for selective ethylene oligomerization and an ethylene oligomerization reaction method. Background technique [0002] With the continuous development of the global economy, the demand for high-performance polyethylene is also increasing. 1-hexene and 1-octene are used as comonomers to prepare polyethylene, and their demand continues to grow at an average annual rate of more than 5.4%. . The main methods for industrial production of 1-hexene and 1-octene include paraffin cracking, ethylene oligomerization and extraction separation, among which ethylene oligomerization is the main method for producing 1-hexene and 1-octene. [0003] US6184428 discloses a nickel catalyst, using a boron compound as an activator, which can catalyze the oligomerization of ethylene to obtain a mixture of linear α-olefins, wherein the content of 1-hexene accounts for 22%, and the conte...
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