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Ziegler-natta catalyst deactivation and neutralization

A Natta catalyst, catalyst technology, applied in the field of deactivation and neutralization, solution polymerization for the production of ethylene polymers, Ziegler-Natta catalyst deactivation and neutralization methods

Pending Publication Date: 2020-11-10
DOW GLOBAL TECH LLC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the use of catalysts to kill components can cause other problems within the polymerization system

Method used

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  • Ziegler-natta catalyst deactivation and neutralization
  • Ziegler-natta catalyst deactivation and neutralization
  • Ziegler-natta catalyst deactivation and neutralization

Examples

Experimental program
Comparison scheme
Effect test

example 1 and comparative example 1

[0053] Example 1 and Comparative Example 1: Catalyst deactivation based on polyoctene test

[0054] The chemical reaction scheme for Example 1 is provided below.

[0055]

[0056] Reactions were performed in an inert atmosphere nitrogen purged glove box. In this glove box, 5.5 mL of 1-octene and 5.5 mL of Isopar-E (manufactured by ExxonMobil Chemical Company) were added to four 40 mL glass vials equipped with magnetic stirring bars. Insert the vial into the insulated slot of the magnetic stirrer block. A thermocouple was inserted through the vial's rubber septum to begin monitoring the temperature. To each of the four vials was added 40 μL of 1.0 M triethylaluminum in hexane (5 equivalents relative to Ti) followed by MgCl 2 Supported Ti-based Ziegler-Natta catalyst solution (8.00 μmol Ti). The vial was immediately sealed with a septum cap and the temperature of the reaction mixture was recorded every five seconds. When the temperature reached 40°C (approximately 10°C e...

example 2

[0058] Example 2: Comparison of HCl neutralization by different metal carboxylates

[0059] The chemical reaction scheme for Example 2 is provided below.

[0060]

[0061] M=Ca, Na, Zn, Mg

[0062] R=C 17 h 35 (stearyl), C 17 h 33 (oil based)

[0063] x=1, 2

[0064] 1 mL of Ziegler-Natta catalyst slurry solution (0.013M Ti) and 9 mL of Isopar-E were added to a 40 mL vial equipped with a stir bar and quenched with 10 mL of deionized water. After stirring at 70 °C for one hour, both the organic and aqueous layers became clear and colorless. The pH of the aqueous layer was acidic as determined by pH paper, indicating the presence of HCl formed in the hydrolysis by the Ziegler-Natta catalyst.

[0065] To neutralize HCl, a solution of the metal carboxylate (0.5, 1.0, 2.0, or 5.0 equivalents relative to the carboxylate) was injected into the vial, and the solution was stirred vigorously at 70 °C for 8 h while continuously monitoring the concentration of the aqueous layer...

example 3 and comparative example 3

[0070] Example 3 and Comparative Example 3: Precipitation Observation After Heating Ziegler-Natta Catalysts and Catalyst Killing Compounds (with and without TEA, 190°C)

[0071] Reactions were performed in a nitrogen purged inert atmosphere glove box. In a glove box, 0.25M calcium stearate, 0.25M zinc stearate and 0.25M magnesium stearate, 0.5M sodium stearate and 0.5M sodium oleate were prepared in Isopar-E. Placed in a 50mL round bottom flask. Additionally, 1 mL of HEC-3 catalyst solution (0.013M Ti) and 20 mL of hexadecane were added. For experiments using triethylaluminum, an additional 5 equivalents of TEA relative to Ti in HEC-3 were added. The solution was heated to 190° C., and then 1 mL of the different catalyst deactivator solution (approximately 250 g catalyst deactivator / g Ti) was added to the flask. Comparative Example 2 included a sample flask with no catalyst deactivator and a flask including calcium stearate as the catalyst deactivator, and Example 3 include...

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Abstract

A solution polymerization process for producing ethylene-based polymer includes introducing ethylene monomer, hydrocarbon solvent, and Ziegler-Natta catalyst into an entrance of a solution polymerization reactor. An ethylene-based polymer is produced by solution polymerizing the ethylene monomer in hydrocarbon solvent. Subsequently, the catalyst deactivator is introduced into the exit of the solution polymerization reactor, thereby producing hydrochloric acid byproduct. The catalyst deactivator includes long chain carboxylate and at least one cation selected from Groups 1, 2, and 12 of the IUPAC periodic table, with the exception of calcium. The catalyst deactivator reduces the effectiveness of the Ziegler-Natta catalyst and neutralizes the hydrochloric acid by forming a chloride salt other than calcium chloride.

Description

[0001] Cross-references to related applications [0002] This application claims priority from U.S. Provisional Patent Application No. 62 / 649,205, filed on March 28, 2018, which is incorporated by reference in its entirety. Technical field [0003] Embodiments of the present disclosure generally relate to the deactivation and neutralization of Ziegler-Natta catalysts. More specifically, embodiments of the present disclosure relate to Ziegler-Natta catalyst deactivation and neutralization in solution polymerization processes for producing ethylene polymers. Background technique [0004] Ethylene polymers are one of the most common plastics and can be used in a variety of ways depending on the structure of the polymer, such as bags / linings, lids / closures, sanitary films, industrial injection molding, etc. It is estimated that approximately 80 million tons of ethylene polymers are produced annually. To meet demand and efficiently produce ethylene polymers, new methods and sy...

Claims

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Application Information

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IPC IPC(8): C08F110/14C08F2/42C08F6/02C08F210/16
CPCC08F2/06C08F2/42C08F6/02C08F110/14C08F210/16C08F2410/08C08F4/6543C08F4/6555C08L23/18C08F110/02C08F210/14C08F2/01C08F10/02
Inventor E·欧阳S·W·埃瓦尔特D·费拉里T·达维迪安R·万斯佩伊布鲁克
Owner DOW GLOBAL TECH LLC
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