Method for preparing aluminosilicate supported irons post-transition metal ethylene polymerization catalyst

A late-transition metal and aluminosilicate technology, which is applied in the field of preparation of iron-based late-transition metal vinyl polymer catalysts, can solve problems such as instability, stickiness, and low apparent density

Inactive Publication Date: 2005-06-29
SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For example, US2002/0187892 A1 introduced the use of Al(Me) 3 or Al(Me) 2 Cl handles the carrier, and then the preparation method of the carrier-type iron-based transition metal catalyst on which the iron-based late transition metal catalyst is loaded, but this method will use extremely unstable Al(Me) 3 or Al(Me) 2 Cl, demanding process requirement

Method used

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  • Method for preparing aluminosilicate supported irons post-transition metal ethylene polymerization catalyst
  • Method for preparing aluminosilicate supported irons post-transition metal ethylene polymerization catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Preparation of the modified carrier: Add 600ml of distilled water to three 1000ml bottles, weigh 30g of artificial sodium-based montmorillonite and slowly add to the three bottles while stirring, and heat. Weigh 10g of cetyltrimethylammonium bromide, dissolve it with a small amount of absolute ethanol, and heat it appropriately. Add hexadecyltrimethylammonium bromide ethanol solution when the artificial sodium montmorillonite distilled water suspension is heated to about 70°C. Mix briskly for about 2 minutes, returning to original mixing speed. At the same time, the temperature was raised to 80° C. and maintained at a constant temperature of 80° C. for about two hours. Then pour out the product, wash it with distilled water until it becomes neutral, filter it with suction, dry it at 80°C, pulverize it with a universal pulverizer, sieve it, and set it aside.

[0030] Loading the iron-based late transition metal complex on the MAO-treated modified montmorillonite: befor...

Embodiment 2

[0033] Preparation of the modified carrier: Add 600ml of distilled water to three 1000ml bottles, weigh 30g of artificial calcium-based montmorillonite, slowly add it to the three bottles while stirring, and heat. Weigh 10g of octadecyltrimethylammonium chloride, dissolve with a small amount of absolute ethanol, and heat appropriately. When the temperature of the artificial calcium-based montmorillonite distilled water suspension is raised to about 80° C., an ethanol solution of octadecyltrimethylammonium chloride is added. Mix briskly for about 2 minutes, returning to original mixing speed. At the same time, the temperature was raised to 90° C. and maintained at a constant temperature of 90° C. for about two hours. Then pour out the product, wash it with distilled water until it becomes neutral, filter it with suction, dry it at 90°C, pulverize it with a universal pulverizer, sieve it, and set it aside.

[0034]Loading the iron-based late transition metal complex on the MAO...

Embodiment 3

[0038] Carrier preparation: same as Example 1.

[0039] Directly load the modified montmorillonite with the iron-based late-transition metal complex: at 25°C, empty the 500ml three-necked flask with nitrogen before the reaction, so that the whole reaction is carried out under the protection of nitrogen. 200ml of heptane was added into the three-necked flask (calcium hydride was refluxed for 24 hours), and 50g of the above-prepared montmorillonite was added under stirring to suspend it uniformly in the heptane solvent. Add dissolved 50mg {[2,6-ArN=C(Me) 2 C 5 h 3 N]FeCl 2}(Ar=2,6-iPr 2 C 6 h 3 ) is the heptane solution of the complex, slowly added dropwise for 2 hours under stirring at normal temperature, and then added 2ml of heptane in the feeding tube, and continued to react for 8 hours at 25° C. under normal pressure. After the reaction, the reaction product was repeatedly washed with heptane under the protection of nitrogen, and stored in a collection bottle in the ...

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Abstract

The invention relates to a catalyst for ethylene synthesis, especially relates to a method for preparing a catalyst of transition metal ethylene synthesis after load; iron system of aluminosilicate, which includes the following steps: a, with agtatering by machine, the aluminosilicate and alcohol solution of long-chain amine salt will react in water in the temperature of 20-90deg.C for 0.5-8hours, wash, dry and scatter it to make modified carrier; b, with agtatering by machine, the modified carrier generated will react with methyl aluxanes in long-chain alkane with the temperature of 0-120deg.C for 0.5-8hours through washing, the activated carrier is made; c, with agtatering by machine, the long-chain alkane solution of complex compound of transition metal after ironis dropped into the activated carrier generated in the temperature of 10-100deg.c, after 0.5-12hours, wash it for several times, the catalyst is made. The invention has high efficiency of loading, simple technique, low cost and the catalyst being made has high activity.

Description

technical field [0001] The invention relates to a catalyst for ethylene polymerization, in particular to a preparation method of an aluminosilicate-loaded iron-based late transition metal ethylene polymer catalyst. Background technique [0002] Iron-based late transition metal catalysts have been widely reported for olefin polymerization. For example, US 6,506,859B1 reported a method for catalyzing olefin polymerization using iron-based late transition metal catalysts and MAO as co-catalysts. However, the polymers prepared by such homogeneous iron-based late-transition metal catalyst systems have poor morphology, low apparent density, and severe sticking to the reactor wall during polymerization, which limits their industrial applications. [0003] In order to solve the above problems, it is an effective way to load iron-based late transition metal catalysts on a carrier to make a supported catalyst. For example, US2002 / 0187892 A1 introduced the use of Al(Me) 3 or Al(Me) ...

Claims

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Application Information

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IPC IPC(8): C08F4/02C08F10/02
Inventor 李三喜韩光唐珅李旭日赵立群
Owner SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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