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Preparation method and application of superhigh-molecular weight polyolefin catalyst

A technology of polyolefin catalyst and main catalyst, which is applied in the fields of olefin polymerization catalyst and olefin polymerization, and can solve problems such as poor reproducibility

Active Publication Date: 2010-12-08
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Domestically produced catalysts catalyze ethylene polymerization to prepare polyethylene with a molecular weight greater than 2 million; however, there are still some technical problems in the preparation of polyethylene catalysts with a molecular weight of 4 million to 6 million, and the reproducibility is poor

Method used

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  • Preparation method and application of superhigh-molecular weight polyolefin catalyst
  • Preparation method and application of superhigh-molecular weight polyolefin catalyst
  • Preparation method and application of superhigh-molecular weight polyolefin catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] In a reactor that has been fully replaced by nitrogen, add activated SiO calcined at 400 ° C 2 1g, 50ml of toluene, stir, control the temperature at about -20°C, add 5ml of n-butyllithium (2.0M hexane solution) dropwise, and react at about 10°C for 1 hour after the dropwise addition; raise the temperature to 40°C and then react for 2 Hour. Reduce to room temperature and filter, wash twice with toluene (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 1 g of dimethyldiethoxy silicon, dropwise add 25 ml of titanium tetrachloride, and react for 1 hour, then slowly (within 4 hours) heat up to 70°C for reaction 2 Hour, stop stirring, leave standstill suspension, layering, extract supernatant liquid, hexane washes four times (each 40 milliliters), vacuum-drying, obtains good fluidity, narrow particle size distribution, spherical procatalyst, The Ti content is 4.5 wt%.

Embodiment 2

[0047] In the reactor that has been fully replaced by nitrogen, add SiO activated by calcination at 500 °C 2 1g, 50ml of toluene, stir, control the temperature at about -30°C, add 0.5g of sodium n-tert-butoxide, react at about 0°C for 1 hour after the dropwise addition; raise the temperature to 50°C for another 3 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 60 ml of n-hexane, cool down to -10°C, add 15g of tetraethoxy silicon, dropwise add 20 ml of titanium tetrachloride, react for 1 hour, slowly (within 4 hours) raise the temperature to 70°C for 2 hours, stop Stir, leave standstill suspension, layering, extract supernatant liquid, hexane washes four times (each 40 milliliters), vacuum-drying, obtains fluidity good, narrow particle size distribution, spherical procatalyst, Ti content is 4.8 wt%.

Embodiment 3

[0049] In a reactor that has been fully replaced by nitrogen, add activated SiO calcined at 600°C 2 1g, 50ml of tetrahydrofuran, stir, control the temperature at about 20°C, add 0.8g of potassium ethoxide, react at about 20°C for 1 hour after the dropwise addition; raise the temperature to 50°C for another 3 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 60 ml of n-hexane, cool down to -10°C, add 20 g of diethoxyisopropoxy tert-butoxy silicon, dropwise add 50 ml of titanium tetrachloride, react for 1 hour, then slowly (within 4 hours) heat up React at 70°C for 2 hours, stop stirring, let the suspension stand, separate layers, extract the supernatant, wash with hexane four times (40 ml each time), and dry in vacuo to obtain a liquid with good fluidity, narrow particle size distribution, and The spherical procatalyst has a Ti content of 5.2 wt%.

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Abstract

The invention relates to a preparation method and application of a superhigh-molecular weight polyolefin catalyst, belonging to the field of olefin polymerization catalysts and olefin polymerization. The preparation method of the catalyst comprises the following steps of: dispersing a carrier in an organic solvent; adding organic lithium or a Grignard reagent and the like in the obtained dispersed solution at -40 DEG C to 30 DEG C, reacting for 0.5-3 hours at -20 DEG C to 30 DEG C after addition, and then raising the temperature to 30-100 DEG C for reacting for 0.5-5 hours to obtain a mixture; filtering and washing the mixture to remove the redundant organic lithium or Grignard reagent; reacting the mixture with a titanium-halogen compound in the organic solvent for 0.5-3 hours at -30 DEG C to 30 DEG C, and then raising the temperature to 30-100 DEG C for reacting for 1-5 hours; and filtering and washing the mixture to remove the redundant titanium-halogen compound and then drying to obtain a main catalyst. The main catalyst prepared in the method has the advantages of favorable particle form, high load capacity, high activity and no drop from the carrier and is suitable for a slurry polymerization process, a gas-phase polymerization process or a combined polymerization process; and the viscosity-average molecular weight of a polymer can be regulated within 800-10000 thousands.

Description

technical field [0001] The invention belongs to the fields of olefin polymerization catalysts and olefin polymerization, and in particular relates to a catalyst for olefin homopolymerization or copolymerization, a preparation method of the catalyst and a preparation method of ultrahigh molecular weight polyolefin. Background technique [0002] Currently published patents on the preparation of ultra-high molecular weight polyethylene catalysts all use MgCl 2 As a carrier, use grinding method, dissolution method and in situ generation carrier MgCl 2 Preparation of catalysts by other methods: Ehlers (US5 587 440) discloses a catalyst and preparation method for preparing ultra-high molecular weight polyethylene with a narrow particle size distribution of polymers. The catalyst is obtained by reducing titanium (IV) halides with organic aluminum compounds and after post-treatment , but the activity of the catalyst is low. Yang Chunbing (CN00819563.3) of Samsung General Chemical ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F10/00C08F4/658C08F4/657C08F4/656C08F4/02C08F10/02
Inventor 黄启谷刘伟娇豆秀丽刘智张新莉杨万泰
Owner BEIJING UNIV OF CHEM TECH
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