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Organic porous material after-supported single cyclopentadienyl chromium catalyst and application thereof

A porous material and post-loading technology, which is applied in the field of organic porous coordination polymer materials, can solve the problems of introducing ash impurities and decreasing catalytic activity, and achieve the effects of high catalytic activity, good stability and high activity

Inactive Publication Date: 2015-09-09
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] As mentioned earlier, this type of catalyst is a homogeneous monochromocene catalyst, which needs to be supported for industrial production, but the support will lead to a decrease in catalytic activity and will introduce ash impurities into the polymer

Method used

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  • Organic porous material after-supported single cyclopentadienyl chromium catalyst and application thereof
  • Organic porous material after-supported single cyclopentadienyl chromium catalyst and application thereof
  • Organic porous material after-supported single cyclopentadienyl chromium catalyst and application thereof

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Experimental program
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Effect test

Embodiment 1

[0036]

[0037] 400 mg (0.66 mmol) of 1,3,5-tris(3-tert-butyl-4-hydroxy-5-formylphenyl)benzene, 182 mg (0.99 mmol) of benzidine and 15 mL of DMSO were added to a 25 ml flask. The reaction mixture was successively reacted in an oil bath at 70°C for 12 hours, at 100°C for one day, and at 120°C for two days. The reaction solution was filtered, and the filter cake was washed with THF, DMF, and CH3OH. The solid was extracted with THF and CH3OH for 6 hours, and then vacuum-dried at 120°C. The obtained orange-yellow solid powder was recorded as Ligand 1, with a yield of 492.6 mg and a yield of 90.1%.

[0038] The synthesis of 1,3,5-tris(3-tert-butyl-4-hydroxy-5-formylphenyl)benzene reference Liu H., Wang M., Wang Y., etal.Synthetic Commun., 2010, 40:1074-1081.

Embodiment 2

[0040]

[0041] 400 mg (0.64 mmol) of 1,3,5-tris(3-phenyl-4-hydroxy-5-formylphenyl)benzene, 182 mg (0.99 mmol) of benzidine and 15 mL of DMSO were added to a 25 ml flask. The reaction mixture was reacted successively in an oil bath at 70°C for 12 hours, at 100°C for one day, and at 120°C for two days. The reaction solution was filtered and washed with THF, DMF, CH 3 OH to wash the filter cake, and the solid was washed with THF, CH 3 OH was extracted by Soxhlet for 6 hours, and then vacuum-dried at 120 °C. The obtained orange-yellow solid powder was recorded as Ligand 2, with a yield of 462.1 mg and a yield of 84.7%.

[0042] The synthesis of 1,3,5-tris(3-phenyl-4-hydroxy-5-formylphenyl)benzene refers to the literature Liu H., Wang M., Wang Y., etal.Synthetic Commun.,2010,40 :1074-1081.

Embodiment 3

[0044]

[0045] Under a nitrogen atmosphere, dissolve 0.16 g of Ligand 1 (containing 0.58 mmol-OH) prepared in Example 1 in 20 mL of anhydrous tetrahydrofuran, add 0.58 mmol of n-butyllithium at -78 ° C, and stir at room temperature for 2 Hour. Add 10 mL tetrahydrofuran solution of 58 mmol / L pentamethyl-substituted monochromocene at -78°C, warm to room temperature, stir for 20 hours, and remove the solvent by filtration. The solid product was washed with dry tetrahydrofuran and dried under vacuum at 140°C for 4 hours. That is, 0.200 g of the organic porous material was obtained to support the metallocene chromium catalyst, which was recorded as complex 1, and the yield was 69.4%. Elemental analysis of its composition: C 73.59%, H 7.62%, N 5.32%. The Cr content measured by ICP was 3.34%. The specific surface area of ​​complex 1 measured by the specific surface area analyzer is 504m 2 / g.

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Abstract

The invention relates to an organic porous material after-supported single cyclopentadienyl chromium catalyst and an application thereof and belongs to the technical field of organic porous coordination polymer materials. The structure expression of the organic porous material after-supported single cyclopentadienyl chromium catalyst is shown in the description. The organic porous material after-supported single cyclopentadienyl chromium catalyst is used as a main catalyst, alkyl aluminum or alkyl aluminum halide or a mixture of alkyl aluminum and alkyl aluminum halide is used as an auxiliary catalyst, and the organic porous material after-supported single cyclopentadienyl chromium catalyst can be used for catalyzing olefin polymerization. The catalyst provided by the invention is good in stability, high in catalytic activity, low in cost and particularly suitable for the preparation of high-molecular weight polyethylene.

Description

technical field [0001] The invention belongs to the technical field of organic porous coordination polymer materials, in particular to the preparation of a single chromocene catalyst supported by an organic porous material and its application in catalyzing ethylene polymerization. Background technique [0002] A large number of studies have proved that in the field of olefin polymerization, the uniqueness of metallocene compounds is that the catalytic performance of metallocene catalysts for polymerization reactions, such as polymerization activity, can be changed by changing the substituents on the ligands of metallocene complexes. , the molecular weight of the polymer and its distribution, etc. to produce a series of high-performance polyolefin products. Metallocene catalysts, with their excellent catalytic performance, have brought huge economic benefits and created rich material wealth in industry, and as a field with complete content and strong theoretical foundation, i...

Claims

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Application Information

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IPC IPC(8): C08F4/6592C08F110/02
Inventor 母瀛许博李贺何江浩李忠平
Owner JILIN UNIV
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