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Synthetic method of metallocene catalyst aid and application of metallocene catalyst aid in 1-decene polymerization process

A metallocene catalyst and technology for synthesis methods, which are applied in chemical instruments and methods, compounds containing elements of Group 3/13 of the periodic table, organic chemistry, etc. The effect of high yield and simple reaction process

Inactive Publication Date: 2019-08-02
镇江巨杰新材料技术研发中心(有限合伙)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

MAO was first discovered and used in the polymerization of α-olefins, but MAO has its own problems, that is, to maintain the high activity of the metallocene catalytic system, MAO as a cocatalyst must be in excess, and the molar ratio of the metallocene compound is usually 100. times, making it limited as a co-catalyst for metallocene catalytic systems

Method used

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Examples

Experimental program
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Embodiment 1

[0032] In a 2L reaction kettle, add 170g of tetrapentafluorophenyl borate and 1120g of dichloromethane, and stir for 30min at room temperature (25°C). 69 g of trityl chloride was added, and the reaction was stirred for 2 hours at a temperature of 25-30° C. in the kettle. Stop the reaction, add 17g of diatomaceous earth, and stir for 10min. After vacuum filtration to remove insoluble solids, the organic phase filtrate was distilled off under reduced pressure to remove most of the solvent dichloromethane. Add 380g of n-heptane, and continue vacuum distillation to remove low-boiling dichloromethane. Vacuum filtration afforded a crude solid. The crude product was vacuum-dried at 50° C. for 10 hours to obtain 200 g of triphenylcarba(pentafluorophenyl) borate as a white powder solid (99% purity, 91.6% molar yield).

Embodiment 2

[0034] In a 2L reaction kettle, add 170g of tetrapentafluorophenyl borate and 1120g of dichloromethane, and stir for 30min at room temperature (25°C). 76.5 g of trityl chloride was added, and the reaction was stirred for 2 hours under the condition that the temperature in the kettle was 25-30°C. Stop the reaction, add 17g of diatomaceous earth, and stir for 10min. After vacuum filtration to remove insoluble solids, the organic phase filtrate was distilled off under reduced pressure to remove most of the solvent dichloromethane. Add 380g of n-heptane, and continue vacuum distillation to remove low-boiling dichloromethane. Vacuum filtration afforded a crude solid. The crude product was vacuum-dried at 50° C. for 10 hours to obtain 208 g of triphenylcarba(pentafluorophenyl) borate as a white powder solid (purity 99%, molar yield 95.3%).

Embodiment 3

[0036] In a 2L reaction kettle, add 170g of tetrapentafluorophenyl borate and 1120g of dichloromethane, and stir for 30min at room temperature (25°C). 51.8 g of N,N-dimethylaniline hydrochloride was added, and the reaction was stirred for 2 hours under the condition that the temperature in the kettle was 25-30°C. Stop the reaction, add 17g of diatomaceous earth, and stir for 10min. After vacuum filtration to remove insoluble solids, the organic phase filtrate was distilled off under reduced pressure to remove most of the solvent dichloromethane. Add 380g of n-heptane, and continue vacuum distillation to remove low-boiling dichloromethane. Vacuum filtration afforded a crude solid. The crude product was vacuum-dried at 50° C. for 10 hours to obtain 178 g of white powder solid N,N-dimethylanilinium tetrakis(pentafluorophenyl) borate (purity 99%, molar yield 93.8%).

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Abstract

The invention discloses a synthetic method of a metallocene catalyst aid and an application of the metallocene catalyst aid in a 1-decene polymerization process. Potassium tetrakis(pentafluorophenyl)borate and trityl chloride (or N,N'-dimethylaniline hydrochloride) react, organic boride trityl tetrakis(pentafluorophenyl)borate (or N,N'-dimethylanilinium tetrakis(pentafluorophenyl)borate) is obtained to serve as the metallocene catalyst aid and successfully applied to a polymerization reaction of 1-decene. The conversion rate of 1-decene reaches 95% or above, the 100 DEG C kinematic viscosity of synthetic polydecene base oil can reach 95 cst or above, and the viscosity index can reach 176. Besides, the synthetic polydecene is uniform in structure and narrow in molecular weight distributionand has dispersity index D between 1.35 and 1.63, that is, the synthetic base oil product has excellent performance and has enormous economic values.

Description

technical field [0001] The invention relates to a synthesis method of a metallocene catalyst auxiliary agent and its application in the polymerization process of 1-decene. [0002] technical background [0003] Poly Alpha Olefin (PAO) is the fourth type of synthetic base oil. As a synthetic base oil, it is different from mineral oil base oil extracted from petroleum by physical distillation. PAO base oil has good viscosity-temperature properties and low-temperature fluidity, and is an ideal base oil for preparing high-grade and special-purpose lubricating oils. PAO is synthesized by polymerization and hydrogenation of α-olefin. If the α-olefin is 1-decene, it is called polydecene. In recent years, lubricating oils have been developed in the direction of no pollution or low pollution, low emissions, low cost, high performance, and energy saving, which to some extent limits the application range of traditional petroleum-based mineral oils, while synthetic lubricating oils Wit...

Claims

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Application Information

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IPC IPC(8): C07F5/02C08F110/14C08F4/6592
CPCC07F5/02C08F110/14C08F4/65927
Inventor 樊爱龙
Owner 镇江巨杰新材料技术研发中心(有限合伙)
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