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Olefin polymerization method

An olefin polymerization and olefin technology, applied in the field of olefin polymerization, can solve the problems of low catalytic efficiency and low efficiency, and achieve the effects of high catalytic activity, stable structure and high catalytic activity

Active Publication Date: 2012-05-16
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0016] The purpose of the present invention is to overcome the catalytic efficiency of the supported metallocene catalyst in the prior art is still low, resulting in the low efficiency of the olefin polymerization reaction using the supported metallocene catalyst, to provide an efficient olefin polymerization method

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preparation example Construction

[0039] The method for preparing the above-mentioned supported metallocene catalyst of the present invention further comprises heating the carrier at a temperature of 300-500°C for 5-20 hours under the protection of an inert gas before loading methylaluminoxane .

[0040] The method for preparing the above-mentioned supported metallocene catalyst of the present invention, for example: may comprise the following steps:

[0041](1) Thermal activation step, calcining the carrier such as rod-shaped SBA-15 at 300-500° C. for 5-20 hours under the protection of nitrogen to obtain a rod-shaped mesoporous material after thermal activation;

[0042] (2) Transfer the thermally activated carrier to a reactor fully replaced by nitrogen, add toluene, methyl aluminoxane, in molar ratio, carrier (calculated as silicon dioxide): toluene: methyl aluminoxane The molar ratio of alkanes is 1:3-10:0.1-1, then stirred at 25-80°C for 1-10 hours, after the completion, washed twice with hexane, and fin...

Embodiment 1

[0054] This example is used to illustrate the supported metallocene catalyst and its preparation method according to the present invention.

[0055] 1) The rod-shaped mesoporous material SBA-15 (commercially purchased from Changchun Jilin University High-tech Co., Ltd., the length of the rod is 30-100 microns, and its pore structure parameters are shown in Table 1) was calcined at 400 ° C for 10 hour (thermal activation), remove hydroxyl group and residual moisture, obtain the rod-shaped mesoporous material after thermal activation;

[0056] 2) Transfer 0.4 g of the thermally activated rod-shaped mesoporous material to a 250 ml glass reactor fully replaced by nitrogen, add 10 ml of refined toluene, methyl aluminoxane (MAO, commercially available from Albemarle, USA) 0.47 g of auxiliary agent was stirred at 50° C. for 4 hours. After completion, wash three times with 20 ml of hexane, and finally dry the solid with nitrogen to obtain an alkylaluminoxane / SBA-15 complex carrier (M...

experiment Embodiment 1

[0066] This experimental example is used to illustrate the catalytic activity of the supported catalyst according to the present invention.

[0067] In a 2-liter stainless steel autoclave, replace three times with nitrogen and ethylene respectively, then add 200 milliliters of hexane solvent, raise the temperature of the kettle to 80 ° C, then add the remaining 800 milliliters of hexane solvent, with the addition of hexane, Add 2 ml of 1 mol / L triethylaluminum (TEA) hexane solution, then add 61.7 mg of SBA-15-YIN-1, feed ethylene to raise and maintain the pressure to 1.0 MPa, and react at 70°C for 1 hour . After the end of the polymerization reaction, the polyethylene particle powder was collected and weighed to obtain 68 grams. The efficiency of the catalyst was 1102gPE / (gcat h) (that is, 2.0×10 7 gPE / (mol Zr h)), bulk density (BD) is 0.285g / ml, melt index: MI 2.16 = 0.0001 g / 10 min.

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Abstract

The invention provides an olefin polymerization method, which comprises the following steps that: under an olefin polymerization condition, one or more than one kind of olefin is contacted with a load type metallocene catalyst, wherein the load type metallocene catalyst comprises a carrier and a metallocene compound and methylaluminoxane which are on the carrier. The olefin polymerization method is characterized in that the carrier is SBA-15, the metallocene compound has a structure shown by the formula 1, M is one of titanium, zirconium and hafnium, and X is halogen. According to the olefin polymerization method, a catalyst with higher catalytic activity is adopted, so that the catalytic efficiency is higher, and further, a larger quantity of polymer can be obtained by using a small quantity of the catalyst.

Description

technical field [0001] The present invention relates to a method for polymerizing olefins. Background technique [0002] The development and application of metallocene catalysts is another major breakthrough in the field of olefin polymerization catalysts after the traditional Ziegler-Natta catalysts. Due to the large amount of methylaluminoxane (MAO) required to achieve high activity of homogeneous metallocene catalysts, the production cost is high, and the obtained polymer has no particle shape, it cannot be used in the widely used slurry method or gas phase polymerization process. use. Moreover, the activity of the metallocene catalyst is very high, and it is prone to localized polymerization at a faster rate during the polymerization reaction, which in turn leads to detonation. [0003] An effective way to solve the above problems is to carry out loading treatment on soluble metallocene catalysts. At present, there are many reports on the supported metallocene catalys...

Claims

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Application Information

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IPC IPC(8): C08F10/00C08F4/6592C08F4/02C08F10/02
Inventor 邱波亢宇王洪涛郭顺郑刚刘长城
Owner CHINA PETROLEUM & CHEM CORP
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