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A kind of magnesium chloride/silica/tetrahydrofuran supported transition metal catalyst and its preparation and application

A post-transition metal and silica technology, which is applied to the application field of the catalyst in the gas phase polymerization or copolymerization of ethylene, can solve the problems of high catalyst loading cost, limited industrial application, complicated preparation method, etc., and achieve good hydrogen adjustment sensitivity Performance and copolymerization performance, high ethylene polymerization catalytic activity, simple preparation method

Active Publication Date: 2016-01-20
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although there are many research reports (PCTInt.Appl.99 / 21898; US6455647; J.Mol.Catal.A2002,188,123; PCTInt.Appl.2004 / 078804) for magnesium chloride compound loaded single-site catalysts, the carrier preparation And the cost of catalyst loading is high, and the particle shape of the carrier is poor and uncontrollable; although the use of spherical magnesium chloride can ensure that the supported catalyst has a good particle shape, the carrier contains components such as alcohol, water, and alkoxy groups, and the preparation of the carrier is complicated. The above shortcomings limit the industrial application of MgCl-supported single-site catalysts
Chinese patent 200910078595.1 provides a method of spray drying to prepare magnesium chloride carrier, and then the carrier is heated, vacuum dried, etc., and then loaded with a transition metal complex. The preparation method of this carrier is also relatively complicated and is not suitable for industrial production.

Method used

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  • A kind of magnesium chloride/silica/tetrahydrofuran supported transition metal catalyst and its preparation and application
  • A kind of magnesium chloride/silica/tetrahydrofuran supported transition metal catalyst and its preparation and application
  • A kind of magnesium chloride/silica/tetrahydrofuran supported transition metal catalyst and its preparation and application

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Experimental program
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Effect test

Embodiment 1

[0030] 1. Preparation of supported catalyst 2,6-bis[1-(2,6-dimethylaniline)ethyl]pyridine ferric dichloride. Under the protection of nitrogen, in a 250mL reactor, add anhydrous magnesium chloride 4.868 g, add 130mL of refined THF, keep the temperature at 70°C, heat and stir for 1 hour. Add 7.510 g of TS-610 silica gel replaced by nitrogen into the reactor, keep the temperature at 30°C, and stir for 1 hour. 0.1937 g of iron homogeneous catalyst 2,6-bis[1-(2,6-dimethylaniline)ethyl]pyridine dichloride was added, and the mixture was stirred at 30°C for 15 minutes. The agitated mother liquor is spray-dried with a spray drying device. The inlet temperature is set to 182°C, the outlet temperature value is 98°C, the pumping speed percentage is 100%, the pump speed percentage is 30%, and the nozzle cleaning frequency is 7 times / min. 8.6219g of the supported catalyst was obtained, the iron content measured by atomic absorption spectrometry was 0.25%, the tetrahydrofuran content measure...

Embodiment 2

[0034] 1. The preparation of supported catalyst 2,6-bis[1-(2,6-dimethylaniline)ethyl]pyridine ferric dichloride

[0035] Under the protection of nitrogen, in a 250 mL reactor, 4.85 g of anhydrous magnesium chloride was added, and 130 mL of refined THF was added, and the mixture was heated and stirred at a constant temperature of 70° C. for 1 hour. Add 7.55 g of TS-610 silica gel replaced with nitrogen into the reactor, keep the temperature at 30°C, and stir for 1 hour. 0.3812 g of iron homogeneous catalyst 2,6-bis[1-(2,6-dimethylaniline)ethyl]pyridine dichloride was added, and the mixture was stirred at 30°C for 15 minutes. The agitated mother liquor was spray-dried with a spray dryer. The inlet temperature was set to 182°C, the outlet temperature was 98°C, the pump speed percentage was 30%, the nozzle cleaning frequency was 7 times / min, and 8.7325g of supported catalyst was obtained. The iron content measured by absorption spectrum was 0.47%, the tetrahydrofuran content determi...

Embodiment 3

[0039] 1. Preparation of supported catalyst 2,6-bis[1-(2,6-diisopropylaniline)ethyl]pyridine ferric dichloride

[0040] Under the protection of nitrogen, in a 250 mL reactor, 4.8703 g of anhydrous magnesium chloride was added, and 130 mL of refined THF was added, and the mixture was heated and stirred at a constant temperature of 70°C for 1 hour. Add 7.5350 g of TS-610 silica gel replaced with nitrogen into the reactor, keep the temperature at 30°C, and stir for 1 hour. Add 0.2145 g of iron homogeneous catalyst 2,6-bis[1-(2,6-diisopropylaniline)ethyl]pyridine ferric dichloride, and stir at 30°C for 15 minutes. The mother liquor after stirring is spray-dried with a spray dryer. The inlet temperature is set to 182°C, the outlet temperature is 98°C, the pumping speed percentage is 100%, the pump speed percentage is 30%, and the nozzle cleaning frequency is 7 times / min. Obtained 8.9930 g of the supported catalyst, the iron content measured by atomic absorption spectroscopy was 0.22%...

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Abstract

The invention relates to a magnesium chloride / silicon dioxide / tetrahydrofuran loaded late transition metal catalyst and a preparation method and application thereof. The preparation method comprises the following steps of: performing reaction between magnesium chloride and a late transition metal complex in an electron donor tetrahydrofuran compound to prepare a matrix; doping the obtained matrix with nanoscale carbon dioxide carrier particles to obtain a suspended liquid; spray drying the obtained suspended liquid to obtain a solid catalyst compound, wherein the molar ratio of magnesium chloride / silicon dioxide / tetrahydrofuran is 0.1-1:0.1-2:5-20, and the weight percentage of central metal M is 0.01-5% in the loaded late transition metal catalyst. The catalyst used for catalyzing copolymerization reaction between ethylene and advanced alpha-olefin is high in copolymerization activity, and obtained resin powder has good particular shape, is high in stacking density, and can be applied to slurry polymerization or vapor phase polymerization process of ethylene.

Description

Technical field [0001] The invention relates to a magnesium chloride / silica / tetrahydrofuran supported post-transition metal catalyst used in the gas phase polymerization or copolymerization process of ethylene and its preparation, and the application of the catalyst in the gas phase polymerization or copolymerization of ethylene. Background technique [0002] The late transition metal olefin polymerization catalyst refers to a catalytic system composed of a late transition metal nickel, palladium, iron, cobalt and other coordination compounds and alkyl aluminum compounds. Late transition metals have been used in the study of olefin polymerization for a long time. However, because late transition metals have a strong tendency to eliminate β-H, most late transition metal catalysts are only suitable for the dimerization or oligomerization of olefins. To high molecular weight olefin polymers. People have tried to use late transition metals to catalyze the polymerization of olefins, ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F10/00C08F10/02C08F4/70C08F4/02
Inventor 何书艳王鹏马建英姜涛王伟众陈开付义曹晨刚赵增辉王立娟邵怀启张丽洋马丽张瑀健关鹏鹏任鹤梁立伟景常荣金毅田炳全
Owner PETROCHINA CO LTD
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