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Preparing method and application of heterogeneous catalyst for olefin polymerization

A technology of heterogeneous catalysts and polyolefin catalysts, which is applied in the field of preparation of heterogeneous catalysts for olefin polymerization, can solve problems affecting the subsequent processing of materials, and achieve the effects of large particle size, high bulk density, and simple preparation methods

Inactive Publication Date: 2019-05-24
NINGBO UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

During polymerization, the carrier is broken due to the huge tension generated by the chain growth, and the broken pieces form nano-scale fragments that remain in the polyolefin matrix, resulting in ash content inside the primary polyolefin particles, which affects the subsequent processing of the material; at the same time, due to the surface of the carrier The acidity and the blocking of active sites on the surface of the carrier make the activity of heterogeneous catalysts only one tenth of that of homogeneous catalysts

Method used

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  • Preparing method and application of heterogeneous catalyst for olefin polymerization
  • Preparing method and application of heterogeneous catalyst for olefin polymerization
  • Preparing method and application of heterogeneous catalyst for olefin polymerization

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] The reaction device was purged with high-purity nitrogen to remove air and water in the reaction device. 900 μmol of polyolefin catalyst TiCl 4 (Ziegler-Natta catalyst) was dissolved in 10 mL of solvent n-heptane, added 10 μmol of additive polysilsesquioxane, and stirred for 1 h, so that the polyolefin catalyst was agglomerated into particles in n-heptane, and a heterogeneous catalyst was prepared solvent. After the heterogeneous catalyst solution is monitored by laser particle size, it is measured that the particle size of the formed particles is 375nm, such as figure 1 shown. Optical microscope pictures of heterogeneous catalyst solutions such as figure 2 shown. Adjust the temperature of the slurry polymerization reactor to 60 °C, add 400 mL of polymerization solvent n-heptane, add 1 mL of the above-mentioned heterogeneous catalyst solution, stir for 10 min, and then add 90 μmol of cocatalyst triethylaluminum (the ratio of cocatalyst and heterogeneous catalyst M...

Embodiment 2

[0026] The reaction device was purged with high-purity nitrogen to remove air and water in the reaction device. 500 μmol of polyolefin catalyst TiCl 3 (Ziegler-Natta catalyst) was dissolved in 10 mL of solvent tetrahydrofuran, and 50 μmol of auxiliary agent diethyl ether (of course, other ethers such as dimethyl ether, silicon ether, and amino ether can also be used as nucleating agents) was stirred for 1 h to make the polyolefin catalyst The tetrahydrofuran is agglomerated into granules, and the heterogeneous catalyst solvent is obtained. After the heterogeneous catalyst solution is monitored by laser particle size, it is measured that the particle size of the formed particles is 50nm. Adjust the temperature of the slurry polymerization reactor to 120 ° C, add 400 mL of polymerization solvent toluene, add 1 mL of the above-mentioned heterogeneous catalyst solution, stir for 1 min, and then add 250 μmol of co-catalyst n-butyllithium (the molar ratio of co-catalyst to heteroge...

Embodiment 3

[0028] The reaction device was purged with high-purity nitrogen to remove air and water in the reaction device. 50mmol of polyolefin catalyst VCl 4 (Ziegler-Natta catalyst) was dissolved in 10 mL of solvent chloroform, and 50 mol of auxiliary agent ethyl acetate was added (of course, other esters such as methyl formate, acrylate, and fatty acid esters could also be used as nucleating agents), and stirred for 1 h to make the poly The olefin catalyst is agglomerated into particles in chloroform to obtain a heterogeneous catalyst solvent. After the heterogeneous catalyst solution is monitored by laser particle size, it is measured that the particle size of the formed particles is 900nm. Adjust the temperature of the slurry polymerization reactor to 0°C, add 400 mL of polymerization solvent n-hexane, add 1 mL of the above-mentioned heterogeneous catalyst solution, stir for 1 min, then add 5 mmol of cocatalyst diethylaluminum chloride (cocatalyst and heterogeneous catalyst The mo...

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Abstract

The invention discloses a preparing method of a heterogeneous catalyst for olefin polymerization. The preparing method is characterized by comprising the following steps of 1, dissolving a polyolefincatalyst into a solvent,wherein the concentration of the polyolefin catalyst in the solvent is 50-5,000 micromole / ml; 2, adding an auxiliary, and conducting stirring to make the polyolefin catalyst agglomerated into particles in the solvent to prepare a heterogeneous catalyst solution, wherein the mole ratio of the polyolefin catalyst to the auxiliary is 10:1,000, and the particle size of the particles is 50-900 nm. The invention further discloses application of the heterogeneous catalyst prepared by means of the preparing method. Compared with the prior art, the preparing method is simple, the prepared heterogeneous catalyst can be used for preparing a polyolefin product with large particle size and high stacking density, and besides, the phenomenon that the wall of a reaction still is sticky cannot occur in the polymerization process; meanwhile, the ultrahigh activity can be obtained even under the ultralow use quantity of a catalyst promoter.

Description

technical field [0001] The invention belongs to the technical field of olefin polymerization, and in particular relates to a preparation method and application of a heterogeneous catalyst for olefin polymerization. Background technique [0002] Catalysts for olefin polymerization mainly include homogeneous catalysts and heterogeneous catalysts. Homogeneous catalysts dissolve catalysts in solvents and carry out catalytic reactions in the form of molecules. Homogeneous catalysis has high activity, however, the prepared polyolefin is very easy to cause the wall sticking phenomenon of the reactor, which affects the continuous production of the process; at the same time, the prepared polyolefin particles have small particle size and low bulk density, which reduces the The value of the product; in addition, in order to obtain a highly active catalyst, a homogeneous catalyst needs to use a large amount of co-catalyst, usually the molar ratio of co-catalyst to catalyst is greater t...

Claims

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Application Information

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IPC IPC(8): C08F110/02C08F110/06C08F110/14C08F136/08C08F4/649C08F4/6592C08F4/80C08F4/78
Inventor 历伟董传鼎
Owner NINGBO UNIV
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