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Preparation method and application of spherical magnesium halide carrier

A technology of magnesium halide and magnesium halide alcohol compound, which is applied in the field of olefin polymerization catalyst carrier and its catalyst and olefin polymerization, can solve the problem of affecting the activity of the catalyst with the amount of titanium loaded, and achieves simple operation, uniform size distribution and high amount of titanium loading. Effect

Active Publication Date: 2012-05-23
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This patent still needs to add a dispersant to the magnesium chloride alcoholate melt to form an emulsion, and the dispersant remaining on the carrier affects the amount of titanium loaded in the catalyst preparation process and the activity of the catalyst

Method used

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  • Preparation method and application of spherical magnesium halide carrier
  • Preparation method and application of spherical magnesium halide carrier
  • Preparation method and application of spherical magnesium halide carrier

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] Preparation of carrier: In a reactor fully replaced by nitrogen, add 1 g of anhydrous MgCl 2 , 10ml of absolute ethanol, stirring, control the temperature at about 120°C for 3 hours, transfer to the mixed solution of 0.3g vacuum ester and 50ml hexane at 30°C while it is hot (120°C), stir for 20min, then let stand and filter, use Wash 3 times with toluene and 3 times with n-hexane (40 ml each time), and vacuum-dry to obtain 2.7 g of spherical magnesium chloride alcoholate carrier.

[0044] Preparation of the main catalyst: In a reactor fully replaced by nitrogen, take 1 g of the carrier obtained above and 10 ml of n-hexane, then cool down to -25°C, add 8ml of titanium tetrachloride dropwise, and keep the temperature at -10°C for 1h, 0 ℃ for 1 hour, 20 ℃ for 1 hour, heated up to 60 ℃ for 2 hours, stop stirring, let the suspension stand, separate layers, remove the supernatant, wash three times with hexane, dry with nitrogen, and get good fluidity, spherical The main cata...

Embodiment 2

[0046] Preparation of carrier: In a reactor fully replaced by nitrogen, add 1 g of anhydrous MgCl 2 , 15ml of absolute ethanol, stirring, control the temperature at about 150°C for 2 hours, transfer to the mixed solution of 3.0g silicone oil and 30ml heptane at 20°C while it is hot (150°C), stir for 60min, then let stand and filter, and use n-hexane Wash with alkane three times (40 ml each time), and dry in vacuo to obtain 2.5 g of spherical magnesium chloride alcoholate carrier.

[0047] Preparation of the main catalyst: In a reactor fully replaced by nitrogen, take 1 g of the carrier obtained above and 10 ml of n-hexane, then cool down to -25°C, add 12ml of titanium tetrachloride dropwise, and keep the temperature at -10°C for 1h, 0 ℃ for 1 hour, 20 ℃ for 1 hour, heated up to 60 ℃ for 2 hours, stop stirring, let the suspension stand, separate layers, remove the supernatant, wash three times with hexane, dry with nitrogen, and get good fluidity, spherical The main catalyst h...

Embodiment 3

[0049] Preparation of carrier: In a reactor fully replaced by nitrogen, add 1 g of anhydrous MgCl 2, 20ml of absolute ethanol, stirring, control the temperature at about 100°C for 3 hours, transfer to a mixed solution of 1.5g of silicon ester and 40ml of hexane at 10°C while it is hot (100°C), stir for 2 hours, then let stand and filter, Wash with n-hexane 3 times (40 ml each time), and dry in vacuum to obtain 2.1 g of spherical magnesium chloride alcoholate carrier.

[0050] Preparation of the main catalyst: In a reactor fully replaced by nitrogen, take 1 g of the carrier obtained above and 10 ml of n-hexane, then cool down to -20 °C, add 20 ml of titanium tetrachloride dropwise, and keep the temperature at -10 °C for 1 h, 0 ℃ for 1 hour, 20 ℃ for 1 hour, heated up to 60 ℃ for 2 hours, stop stirring, let the suspension stand, separate layers, remove the supernatant, wash three times with hexane, dry with nitrogen, and get good fluidity, spherical The main catalyst has a Ti c...

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Abstract

The invention belongs to the fields of olefin polymerization catalyst carriers and catalysts thereof and olefin polymerization. A preparation method of a spherical catalyst carrier comprises the steps of: adding alcohol and magnesium halide in a mol ratio of 2-100:1 into a closed container, raising the temperature to 60-180 DEG C, stirring for reacting for 10min-6h; transferring the obtained solution to an inert solvent or a mixed system of the inert solvent and an emulsifying agent while the solution is hot, wherein the inert solvent or the mixed system of the inert solvent and the emulsifying agent has a temperature of -25 DEG C-30 DEG C and is in a flowing state; stirring, and washing 3-6 times with an organic solvent; and vacuum drying to obtain a solid spherical magnesium halide alcohol compound particle with small carrier particle diameter and uniform distribution, wherein the particle diameter of the carrier is 2 mu m-30 mu m. The carrier is dispersed into an organic solvent and reacts with a titanium halide compound at a temperature of -30 DEG C-30 DEG C to obtain a master catalyst. The master catalyst has spherical particles; and the titanium loading quantity (4.0-9.76 percent by weight) is high, the efficiency on catalyzing vinyl polymerization or propene polymerization or olefin polymerization by the catalyst is high and the average molecular weight of polyolefin can be adjusted between 15,000 and 9,000,000.

Description

technical field [0001] The invention belongs to the field of olefin polymerization catalyst carrier, its catalyst and olefin polymerization, and specifically relates to a spherical magnesium halide carrier for ethylene polymerization, propylene polymerization or olefin copolymerization, a spherical magnesium halide carrier catalyst and a preparation method. Background technique [0002] The preparation method of the early supported catalyst is usually to co-grind the magnesium compound and the titanium halide, or to grind the magnesium compound and then treat it with the titanium halide. A large amount of fine powder is produced in the process of polyolefin, which brings many difficulties to the production of polyolefin. When spherical magnesium chloride is used as a carrier, spherical catalyst particles can be obtained. This spherical granular catalyst can synthesize spherical olefin polymers that are similar in shape to the catalyst and have good fluidity and bulk density....

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F4/02C08F10/02C08F10/06C08F10/00
Inventor 黄启谷刘伟娇豆秀丽张新莉孔媛杨万泰
Owner BEIJING UNIV OF CHEM TECH
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