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Catalyst for ethylene oligomerization and preparation method thereof

A technology of ethylene oligomerization and catalyst, applied in the field of ethylene oligomerization catalyst and its preparation, to achieve the effects of simplified post-treatment process, high selectivity and avoiding elution

Active Publication Date: 2017-03-15
TIANJIN UNIVERSITY OF SCIENCE AND TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Patent CN 101041610A discloses a homogeneous catalyst for the preparation of α-olefins by ethylene oligomerization of substituted phenylpyridyl monoimine iron complexes. The catalyst has high selectivity to octene-1 and hexene-1 with high added value High, but low selectivity to butene-1 with low added value

Method used

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  • Catalyst for ethylene oligomerization and preparation method thereof
  • Catalyst for ethylene oligomerization and preparation method thereof
  • Catalyst for ethylene oligomerization and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] (1) Synthesis of PNP ligand: take 7.02ml (30.0mmol) aminopropyltriethoxysilane (APTES) and 9.19ml (66.0mmol) triethylamine (NEt 3 ) in a round-bottom bottle with a branched mouth, and protect it with nitrogen, add 120ml of toluene, and stir at -40°C. After stirring evenly, slowly drop diphenyl phosphorus chloride (Ph 2 PCl) 11.14ml (60.0mmol) to room temperature (dropping time 1.5h), after stirring at room temperature for 2h, press filter to obtain the liquid part, and wash the solid three times with a mixed solvent of 20ml toluene and 20ml ether each time. The liquids were collected together, vacuum-dried, and finally recrystallized three times with treated ethanol to obtain the final white powder, which is the desired PNP ligand.

[0032] (2) Grafting of PNP ligands on molecular sieves: Take 5.00 g of mesoporous molecular sieves MCM-41 and 1.00 g of PNP ligands after vacuum drying (100 ° C, -0.1 MPa, 10 h) in a nitrogen-protected reaction flask, add toluene , the mo...

Embodiment 2

[0036] (1) Synthesis of PNP ligand: take 7.02ml (30.0mmol) aminopropyltriethoxysilane (APTES) and 9.19ml (66.0mmol) triethylamine (NEt 3 ) in a round-bottom bottle with a branched mouth, and protect it with nitrogen, add 120ml of toluene, and stir at -40°C. After stirring evenly, slowly drop diphenyl phosphorus chloride (Ph 2 PCl) 11.14ml (60.0mmol) to room temperature (dropping time more than 1h), after stirring at room temperature for 2h, press filter to obtain the liquid part, and wash the solid three times with a mixed solvent of 20ml toluene and 20ml ether each time. The liquids were collected together, vacuum-dried, and finally recrystallized three times with treated ethanol to obtain the final white powder, which is the desired PNP ligand.

[0037] (2) Grafting of PNP ligands on molecular sieves: Take 5.00 g of mesoporous molecular sieve SBA-151.00 g of PNP ligands after vacuum drying (100 ° C, -0.1 MPa, 10 h) in a nitrogen-protected reaction flask, add toluene, toluen...

Embodiment 3

[0041] (1) Synthesis of PNP ligand: take 7.02ml (30.0mmol) aminopropyltriethoxysilane (APTES) and 9.19ml (66.0mmol) triethylamine (NEt 3 ) in a round-bottom bottle with a branched mouth, and protect it with nitrogen, add 120ml of toluene, and stir at -40°C. After stirring evenly, slowly drop diphenyl phosphorus chloride (Ph 2 PCl) 11.14ml (60.0mmol) to room temperature (dropping time more than 1h), after stirring at room temperature for 2h, press filter to obtain the liquid part, and wash the solid three times with a mixed solvent of 20ml toluene and 20ml ether each time. The liquids were collected together, vacuum-dried, and finally recrystallized three times with treated ethanol to obtain the final white powder, which is the desired PNP ligand.

[0042] (2) Grafting of PNP ligands on molecular sieves: take 5.00 g of microporous molecular sieve NaY 1.00 g of PNP ligands after vacuum drying (100 ° C, -0.1 MPa, 10 h) in a nitrogen-protected reaction flask, add toluene, and the...

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Abstract

The invention relates to a catalyst for ethylene oligomerization and a preparation method thereof. The catalyst comprises a main catalyst which is a catalyst obtained by the steps of taking molecular sieve as a carrier, carrying out chemical bond grafting of silicon hydroxyl on the molecular sieve surface and a bis(diphenylphosphino)ammonia ligand containing silicon ethoxy, and then complexing with a chromium active component. The invention also provides the preparation method of the catalyst. The catalyst has the advantages of high catalytic activity, easy separation from a product and high content of alpha-olefins in the oligomerization product when used for catalyzing ethylene oligomerization.

Description

technical field [0001] The invention belongs to the field of ethylene oligomerization catalysts, and relates to a Cr-based catalyst, in particular to a catalyst for ethylene oligomerization and a preparation method thereof. Background technique [0002] As an important chemical product and intermediate, linear α-olefins are mainly used in ethylene comonomers, plasticizers, fatty acids, detergents, and intermediates of lubricating oil additives and lubricating oil additives. Among them, as a comonomer of ethylene, it can significantly increase the mechanical properties, optical properties, tear strength and impact strength of polyethylene. With the continuous development of the polyolefin industry, the demand for α-olefins is also increasing worldwide. Ethylene oligomerization is the main method for obtaining α-olefins, and its reaction catalysts mainly include nickel-based, chromium-based, zirconium-based and aluminum-based. [0003] Patent CN1566041A discloses a method fo...

Claims

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Application Information

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IPC IPC(8): B01J31/24C07C2/36C07C11/02
CPCB01J31/2457B01J2231/20B01J2531/0205B01J2531/62C07C2/36C07C11/02Y02P20/52
Inventor 邵怀启宋立武王晶晶姜涛陈延辉
Owner TIANJIN UNIVERSITY OF SCIENCE AND TECHNOLOGY
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