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Supported olefin polymerization catalyst

A catalyst and carrier technology, applied in the field of catalysts and their preparation, can solve problems such as loss of activity and failure

Inactive Publication Date: 2002-06-05
EQUSR CHEM LP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

U.S. Patents 5,554,775 and 5,539,124 describe that these catalysts should be used as soon as they are prepared because their activity will be lost with storage
Furthermore, our own initial studies using untreated supports to prepare supported heterometallocenes were largely unsuccessful (see Comparative Example 8 and Table 6 below)

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Example 1: Catalysts supported on silica treated with trimethyl borate extend the shelf life

[0041] Catalyst preparation

[0042] Catalyst 1A: Silica (Davison 948, 10-20 grams) was placed in a quartz tube with a sinter used as a gas distributor plate. Nitrogen is used to fluidize the silica in the tube. The quartz tube was placed in a heating furnace, and the silica was heated at 150°C for 4 hours. The tube was then heated to 250°C in 1 hour and then cooled to 150°C. A syringe was used to add trimethyl borate (1.6 mmol / g silica after correction for 5% volatilization in silica) into the fluidized bed. The silica in the fluidized bed was fluidized for 2 hours, and then cooled and discharged into a storage container under a nitrogen atmosphere.

[0043] The cyclopentadienyl (1-methyl borate benzene) · zirconium dichloride (0.046 g, 0.12 mmol / g SiO 2 ) And trityl tetrakis (pentafluorophenyl) borate (0.13 g, 0.14 mmol / g SiO 2 ) Was dissolved in toluene (5 ml) under a nitrogen ...

Embodiment 2

[0048] Example 2: Catalyst supported on HMDS treated silica

[0049] Catalyst preparation

[0050] Catalyst 2A:

[0051] Pure hexamethyldisilylamine (HMDS) in an amount equivalent to 12.5 (weight)% of the silica was slowly added to the stirring silica. After treatment, silica generally contains 4.0-4.2% carbon. The HMDS treated silica is dried in a fluidized bed dryer at 600°C under a stream of dry nitrogen for 6 hours before storage.

[0052] In a dry box with an inert atmosphere (nitrogen), the HMDS-treated silica (2.0 g) was transferred to a three-necked flask equipped with a gas inlet tube, overhead stirrer and rubber septum. In another vial, mix bis(1-methyl borate benzene) zirconium dichloride (0.034 g, 0.10 mmol) and trityl tetrakis(pentafluorophenyl) borate (0.111 g, 0.12 mmol) Mol) was dissolved in dry toluene (2 mL). The vial is sealed with a rubber septum. The catalyst / co-catalyst solution was then added dropwise to the treated silica via a syringe with rapid stirring, ...

Embodiment 3

[0058] Example 3: The catalyst supported on silica treated with HMDS extends the shelf life

[0059] Catalyst preparation

[0060] Catalyst 3: Except that cyclopentadienyl (1-borate benzene) · zirconium dichloride (0.032 g, 0.010 mmol) is used instead of bis (1-borate benzene) · zirconium dichloride, the rest The step of preparing catalyst 2A is carried out.

[0061] Aggregation test

[0062] The polymerization reaction was carried out in a 1-liter stainless steel high-pressure reactor. Hydrogen (0.7 mmol) was introduced into the reactor from a 50 ml vessel, and the amount of hydrogen added was determined by measuring the pressure difference of the vessel. Triethylaluminum (0.38 mmol; 2.3 mL of 0.1 molar heptane solution) was added to a reactor filled with isobutane (approximately 500 mL), the temperature had reached 75°C and was equilibrated. Ethylene was added to the reactor (to a pressure of 400 psig), followed by a mixture of supported catalyst and 1.5 milliliters of triethyl ...

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PUM

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Abstract

A supported olefin polymerization catalyst system and a method of making it are disclosed. The catalyst system comprises: (a) a support chemically treated with an organoaluminum, organosilicon, organomagnesium, or organoboron compound; (b) a single-site catalyst that contains a polymerization-stable, heteroatomic ligand; and (c) an activator. Chemical treatment is a key to making supported heterometallocenes that have high activity and long shelf-lives, and can effectively incorporate comonomers.

Description

Invention field [0001] The invention relates to a supported catalyst for olefin polymerization and a preparation method thereof. The catalyst comprises a support treated with an effective amount of a chemical modifier, at least one polymerization-stable, anionic, heteroatom ligand single-site catalyst and an activator. The modifier is organic aluminum, organic silicon, organic magnesium or organic boron compound. Background of the invention [0002] Many olefin polymerization catalysts including conventional Ziegler-Natta catalysts are well known. Although these catalysts are low in price, their activity is low, and the polymers produced have a narrow-medium molecular weight distribution (Mw / Mn>4), and usually have poor copolymerization with α-olefins. In order to improve polymer performance, high-activity single-site catalysts, especially metallocenes, have begun to replace Ziegler-Natta catalysts. Although the price is relatively high, this novel cataly...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/02B01J31/14B01J31/16B01J31/22B01J37/02B01J37/03C08F4/02C08F4/64C08F4/642C08F4/646C08F4/659C08F4/6592C08F10/00C08F110/02C08F210/16
CPCB01J31/1616B01J2531/0225B01J31/0274B01J31/0231C08F10/00C08F210/16B01J2531/46C08F4/6592C08F4/65908C08F110/02B01J31/165B01J2531/0236B01J2531/0233B01J31/0272C08F4/65912B01J31/0275B01J31/2295B01J31/14B01J2531/48C08F4/65916C08F210/08C08F210/14
Inventor 王哨天B·P·艾瑟顿K·E·梅尔M·W·林驰L·N·温斯劳L·V·克里布斯刘家礎
Owner EQUSR CHEM LP
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