Olefin polymerization method

A technology of olefin polymerization and compounds, applied in the field of olefin polymerization, can solve the problems of complex reaction by-products, carrier adhesion, low polymer bulk density, etc., and achieve good particle shape effect

Active Publication Date: 2017-05-10
黑龙江省龙油石油化工股份有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the composite spherical carrier is easy to stick during the preparation process, and it is difficult to form spherical particles with suitable particle size.
[0003] In the prior art, the methods for preparing catalysts for olefin polymerization mainly include: ① first prepare the carrier by reacting the magnesium halide alcoholate with ethylene oxide compounds, and then directly add the magnesium halide alcoholate to the In the reactor of ethylene oxide compounds, the catalyst carrier prepared by this method has the disadvantages of unstable preparation process, easy carrier adhesion, and poor carrier molding effect.
② Use epoxide and tributyl phosphate compounds to dissolve magnesium chloride to form a uniform solution, and then use titanium tetrachloride to precipitate t

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0044] Example 1

[0045] (1) Preparation of carrier

[0046] In a 500ml reactor, add 150ml of white oil, 30g of magnesium chloride, 50ml of absolute ethanol, 2.0g of diethoxymagnesium and 0.012g of sodium chloride, and raise the temperature to 125°C under stirring. After 2 hours of constant temperature reaction, a liquid mixture was obtained.

[0047] Press the liquid mixture into 300ml of methyl silicone oil preheated to 125°C, stir and emulsify at high speed (1600rpm) for 30min.

[0048] The emulsified product is introduced into a 2L hexane solution previously cooled to -35°C, and after rapid cooling, it is dispersed into small droplets of MgCl 2 The alcohol compound melt becomes spherical particles after cooling and solidification. The liquid was removed by filtration, and the solid was washed 5 times with 300 ml of hexane, and dried under vacuum at 30° C. for 1 hour to obtain a solid support of magnesium chloride alcoholate.

[0049] Through infrared spectroscopy and 1 After HNMR...

Example Embodiment

[0058] Example 2

[0059] (1) Preparation of carrier

[0060] In a 500ml reactor, add 150ml of white oil, 30g of magnesium chloride, 50ml of absolute ethanol, 4.0g of diethoxymagnesium and 0.012g of sodium chloride, and raise the temperature to 125°C with stirring. After 2 hours of constant temperature reaction, a liquid mixture was obtained.

[0061] Press the liquid mixture into 300ml of methyl silicone oil preheated to 125°C, stir and emulsify at high speed (1600rpm) for 30min.

[0062] The emulsified product is introduced into a 2L hexane solution previously cooled to -35°C, and after rapid cooling, it is dispersed into small droplets of MgCl 2 The alcohol compound melt becomes spherical particles after cooling and solidification. The liquid was removed by filtration, and the solid was washed 5 times with 300 ml of hexane, and dried under vacuum at 30° C. for 1 hour to obtain a solid support of magnesium chloride alcoholate.

[0063] Through infrared spectroscopy and 1 After HNMR ...

Example Embodiment

[0067] Example 3

[0068] (1) Preparation of carrier

[0069] In a 500ml reactor, add 150ml of white oil, 30g of magnesium chloride, 50ml of absolute ethanol, 2.0g of diethoxymagnesium and 0.015g of manganese chloride, and heat to 125°C under stirring. After 2 hours of constant temperature reaction, a liquid mixture was obtained.

[0070] Press the liquid mixture into 300ml of methyl silicone oil preheated to 125°C, stir and emulsify at high speed (1600rpm) for 30min.

[0071] The emulsified product is introduced into a 2L hexane solution previously cooled to -35°C, and after rapid cooling, it is dispersed into small droplets of MgCl 2 The alcohol compound melt becomes spherical particles after cooling and solidification. The liquid was removed by filtration, and the solid was washed 5 times with 300 ml of hexane, and dried under vacuum at 30° C. for 1 hour to obtain a solid support of magnesium chloride alcoholate.

[0072] (2) Preparation of catalyst for olefin polymerization: The m...

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Abstract

The invention relates to an olefin polymerization method. The method comprises steps as follows: a hexane solution of triethyl aluminum, a hexane solution of cyclohexyldimethoxymethylsilane and a catalyst are sequentially added to a high-pressure reactor under the protection of nitrogen, the high-pressure reactor is closed, 1.5-8.0 L of hydrogen and liquid olefin are added, the components are heated to 60-80 DEG C to react for 1-2 h, cooled, subjected to pressure release, discharged and dried, and polymers are obtained. According to the olefin polymerization method, a supporter and the catalyst are improved, so that when the catalyst prepared from the supporter is used for polymerization of olefin, especially, polymerization of propylene, activity and hydrogen regulation sensitivity of the catalyst can be improved, particle morphology of obtained polymers is good, bulk density of the polymers can be reduced, and no special-shaped materials are produced basically.

Description

technical field [0001] The invention belongs to the field of organic chemical synthesis, in particular to an olefin polymerization method. Background technique [0002] In the polymerization of olefins, catalysts are often required for catalysis. At present, Ziegler-Natta catalysts for olefin polymerization are basically prepared by loading titanium halides on supports. The carrier commonly used in the preparation of Ziegler-Natta catalysts is magnesium chloride alcoholate, and its overall performance is superior to catalysts prepared by other carriers. The preparation of carrier magnesium chloride alcoholate generally adopts methods such as spray drying, spray cooling, high-pressure extrusion, high-speed stirring, emulsification molding, and high-gravity rotating bed. However, in the process of catalyzing the polymerization of olefins, the catalyst prepared by the carrier obtained by this method is prone to breakage of polymer particles, resulting in excessive fine powder...

Claims

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Application Information

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IPC IPC(8): C08F10/00C08F10/06C08F110/06C08F4/02C08F4/649C08F4/646
CPCC08F10/00C08F10/06C08F110/06C08F4/022C08F4/6494C08F4/6465C08F2500/15C08F2500/12C08F2500/18
Inventor 王磊王振国陈雪
Owner 黑龙江省龙油石油化工股份有限公司
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