Catalyst used for olefin polymerization and preparation method thereof

An olefin polymerization and catalyst technology, applied in the field of olefin polymerization catalyst and its preparation, can solve the problems of complex reaction by-products, low polymer bulk density, and difficulty in forming spherical particles of particle size and size, and achieves good particle shape and hydrogen regulation. The effect of high sensitivity and low fines content

Active Publication Date: 2017-06-13
营口风光新材料股份有限公司
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  • Summary
  • 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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  • Catalyst used for olefin polymerization and preparation method thereof
  • Catalyst used for olefin polymerization and preparation method thereof
  • Catalyst used for olefin polymerization and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] (1) Preparation of carrier

[0046] In a 500ml reaction kettle, add 150ml of white oil, 30g of magnesium chloride, 50ml of absolute ethanol, 2.0g of diethoxymagnesium and 0.012g of sodium chloride, heat up to 125°C under stirring, and react at a constant temperature for 2 hours to obtain a liquid mixture.

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

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

[0049] by infrared spectroscopy and 1 After HNMR nuclear magnetic measurement and analysis,...

Embodiment 2

[0057] (1) Preparation of carrier

[0058] In a 500ml reaction kettle, add 150ml of white oil, 30g of magnesium chloride, 50ml of absolute ethanol, 4.0g of diethoxymagnesium and 0.012g of sodium chloride, heat up to 125°C under stirring, and react at a constant temperature for 2 hours to obtain a liquid mixture.

[0059] Press the liquid mixture into 300ml of methyl silicone oil preheated to 125°C, and stir at high speed (1600rpm) to disperse and emulsify for 30min.

[0060] Introduce the emulsified product into 2L hexane solution pre-cooled to -35°C, and after rapid cooling, disperse into small droplets of MgCl 2 After the alcoholate melt is cooled and solidified, it becomes spherical particles. The liquid was removed by filtration, the solid was washed 5 times with 300 ml of hexane, and vacuum-dried at 30° C. for 1 hour to obtain a solid carrier of magnesium chloride alcoholate.

[0061] The composition of the obtained magnesium halide adduct is {MgCl 2 ·[Mg(OEt) 2 ] 0...

Embodiment 3

[0065] (1) Preparation of carrier

[0066] In a 500ml reaction kettle, add 150ml of white oil, 30g of magnesium chloride, 50ml of absolute ethanol, 2.0g of diethoxymagnesium and 0.015g of manganese chloride, heat up to 125°C under stirring, and react at constant temperature for 2 hours to obtain a liquid mixture.

[0067] Press the liquid mixture into 300ml of methyl silicone oil preheated to 125°C, and stir at high speed (1600rpm) to disperse and emulsify for 30min.

[0068] Introduce the emulsified product into 2L hexane solution pre-cooled to -35°C, and after rapid cooling, disperse into small droplets of MgCl 2 After the alcoholate melt is cooled and solidified, it becomes spherical particles. The liquid was removed by filtration, the solid was washed 5 times with 300 ml of hexane, and vacuum-dried at 30° C. for 1 hour to obtain a solid carrier of magnesium chloride alcoholate.

[0069] (two) preparation is used for the catalyst of olefin polymerization: method is the s...

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Abstract

The invention relates to a catalyst used for olefin polymerization and a preparation method thereof. The preparation method is as follows: in a reactor, under the protection of nitrogen, adding an organic solvent and a titanium compound, cooling to-30 to-10 DEG C, adding a carrier, maintaining at-30 to-10 DEG C, and stirring for 30-40min; slowly heating to 100 to 120 DEG C, in the heating process, adding an electron donor compound, reacting at 100-120 DEG C for 30-40min, filtering a liquid, again adding the titanium compound, heating to 110 to 130 DEG C, maintaining at 110 to 130 DEG C for 30-40min, filtering the liquid, washing an obtained solid, and drying under vacuum to obtain a target product. In a magnesium halide alcohol adduct formation process, a forming agent and a particle form control agent are added, the particle size distribution of the obtained carrier is more concentrated, the carrier is used for preparing the catalyst, activity and hydrogen sensitivity of the catalyst can be improved when the carrier is used for olefin polymerization especially for propylene polymerization, the bulk density of an obtained polymerization product is moderate, and the polymerization product is basically free of abnormity materials.

Description

technical field [0001] The invention belongs to the field of catalysts, in particular to a catalyst for olefin polymerization and a preparation method thereof. Background technique [0002] 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. Although people try to add an electron donor compound i...

Claims

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Application Information

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IPC IPC(8): C08F10/00C08F4/646C08F4/02C08F110/06
CPCC08F10/00C08F110/06C08F4/022C08F4/6465C08F2500/15C08F2500/12C08F2500/18
Inventor 王磊王振国陈雪
Owner 营口风光新材料股份有限公司
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