Loading method of polyolefin catalyst

A polyolefin catalyst and carrier technology, applied in the field of olefin polymerization catalyst and olefin polymerization, can solve the problems of low catalyst loading, small catalyst loading, poor polymer shape, etc., and achieve good particle shape, good particle shape, and equipment. less demanding effects

Active Publication Date: 2010-01-27
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are still problems such as small catalyst loading and low catalytic efficiency, especially the gas phase polymerization catalyst of ethylene, which is mainly based on SiO 2 As a carrier, the catalyst loading is low
Although metallocene catalysts and non-metallocene catalysts can efficiently catalyze olefin solution polymerization, there are still

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] In a reactor fully replaced with nitrogen, add 1 g of activated SiO 2 , 50ml of tetrahydrofuran, stirring, controlling the temperature at about 0°C, adding 5ml of n-butyllithium (2.0M hexane solution) dropwise, and reacting at about 0°C for 1 hour after the dropwise addition; heating to 40°C for another 2 hours. Reduce to room temperature and filter, wash twice with tetrahydrofuran (40 ml each time), and wash twice with n-hexane (40 ml each time). Add 50 ml of n-hexane, cool down to -25°C, add 10 ml of titanium tetrachloride dropwise, react for 1 hour, then slowly (within 4 hours) raise the temperature to 60°C for 2 hours, stop stirring, let the suspension stand, and divide layer, extract the supernatant, wash with hexane four times (40 milliliters each), and dry in vacuo to obtain a spherical supported catalyst with good fluidity, narrow particle size distribution. The Ti content was determined to be 4.5 wt% by atomic absorption method.

Embodiment 2

[0038] In a reactor fully replaced with nitrogen, add 1 g of activated SiO 2 , add 40 milliliters of n-hexane, add 2 milliliters of diethylaluminum chloride (2.0 M), and react at 30° C. for 2 hours. Filter, wash twice with n-hexane solvent, and filter. Add 50ml of tetrahydrofuran, stir, control the temperature at about 0°C, add 5ml of n-butyllithium (2.0M hexane solution) dropwise, and react at about 0°C for 1 hour after the dropwise addition; raise the temperature to 40°C for another 2 hours. Reduce to room temperature and filter, wash twice with tetrahydrofuran (40 ml each time), and wash twice with n-hexane (40 ml each time). Add 50 ml of n-hexane, cool down to -20°C, add 10 ml of titanium tetrachloride dropwise, and react for 1 hour, then slowly (within 4 hours) heat up to about 55°C for 2 hours, stop stirring, and let the suspension stand. Separate layers, extract the supernatant, wash with hexane four times (40 ml each time), and dry in vacuum to obtain a spherical sup...

Embodiment 3

[0040] In a reactor fully replaced with nitrogen, add 1 g of activated SiO 2 , toluene 50ml, stirring, control temperature is about 10 ℃, dropwise add n-butyllithium (2.0M hexane solution) 5 ml, react for 1 hour; heat up to 40 ℃ for about 2 hours. Reduce to room temperature and filter, wash twice with tetrahydrofuran (40 ml each time), and wash twice with n-hexane (40 ml each time). Add 50 ml of n-hexane, cool down to -20°C, add 10 ml of titanium tetrachloride dropwise, react for 0.5 hours, then slowly (within 3.5 hours) heat up to about 55°C and react for 2 hours, stop stirring, and let the suspension stand. Separate layers, extract the supernatant, wash with hexane four times (40 ml each time), and dry in vacuum to obtain a spherical supported catalyst with good fluidity, narrow particle size distribution. The Ti content was determined to be 3.8wt% by atomic absorption method.

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PUM

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Abstract

The invention belongs to the field of a polyolefin catalyst. The method comprises the steps: dissolving or suspending a carrier in an organic solvent; adding compounds of organic lithium, organic sodium or organic potassium or a format reagent to the obtained carrier liquor or suspending liquor at the temperature of -40 DEG C to 30 DEG C; reacting for 0.5 to 3 hours at the temperature of -20 DEG C to 10 DEG C after the adding step; raising the temperature to 30 DEG C to 80 DEG C; reacting for 0.5 to 3 hours; obtaining a mixture; filtering the mixture for washing and removing residual organic lithium, organic sodium, organic potassium or the format reagent; reacting with titanium, metallocene, non-metallocene, vanadium, rare earth metal or chromic halide in the organic solvent at the temperature of -40 DEG C to 30 DEG C; reacting for 0.5 to 3 hours at the temperature of -30 DEG C to 0 DEG C after the adding step; raising the temperature to 20 DEG C to 100 DEG C; reacting for 1 to 5 hours; removing the residual halide by filtering and washing; drying; and obtaining a solid catalyst. The catalyst has the advantages of good grain shape, high loading quantity and high activity, does not fall off the carrier and is suitable for vapor phase polymerization technology, slurry polymerization technology or combination polymerization technology.

Description

technical field [0001] The invention belongs to the fields of olefin polymerization catalysts and olefin polymerization, and in particular relates to a catalyst loading method for homopolymerization or copolymerization of olefins. Background technique [0002] Olefin polymerization catalyst is the core of polyolefin polymerization technology. The catalytic efficiency of traditional Ziegler-Natta catalyst loaded on the carrier is significantly improved, which is called high-efficiency Ziegler-Natta catalyst, which makes the polyolefin industry develop rapidly. However, there are still problems such as small catalyst loading and low catalytic efficiency, especially the gas phase polymerization catalyst of ethylene, which is mainly based on SiO 2 As a carrier, the catalyst loading is low. Although metallocene catalysts and non-metallocene catalysts can efficiently catalyze olefin solution polymerization, there are still many engineering problems in industrial production, such...

Claims

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Application Information

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IPC IPC(8): C08F4/02C08F4/646C08F4/649C08F10/00
Inventor 黄启谷汪红丽孔媛豆秀丽刘伟娇杨万泰
Owner BEIJING UNIV OF CHEM TECH
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