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Montmorillonite-TiCl4 catalyst and process for preparing polyolefin/montmorillonite composition

A technology of titanium tetrachloride and composite materials, applied in physical/chemical process catalysts, chemical instruments and methods, chemical/physical processes, etc., can solve problems such as cost increase, consumption, reduction of metallocene catalyst activity, etc., and achieve easy industrial production effect

Inactive Publication Date: 2002-01-09
CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method has the following disadvantages: 1) freeze-drying process clay increases the cost, and is time-consuming, 2) consumes a large amount of expensive MAO, [MAO] / [Ti] molar ratio is 1000~>3000, 3) the activity of metallocene catalyst Greatly reduced

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Under nitrogen protection, 2.5 grams of magnesium dichloride MgCl 2 , was added to 100ml of refined butanol and stirred at 60°C for 2 hours to form a uniform transparent solution, and the insoluble impurities were filtered off. to MgCl 2 - Add 10 grams of sodium montmorillonite calcined at 400° C. to the butanol solution, continue stirring at 60° C. for 2 hours, then filter off excess butanol, and wash the solid product three times with 50 ml of dry hexane. Add 100ml of dry hexane to the reaction system, and add 10mmol of triisobutylaluminum Al(i-C 4 h 9 ) 3 , continue to react for 30 minutes, then filter and wash 3 times with 50ml of dry hexane. Add 100ml titanium tetrachloride TiCl to the reaction system 4 , stirred at 80 °C for 2 h, filtered off the excess TiCl 4 Finally, the solid product was washed 5 times with 50 ml of dry hexane, and dried under reduced pressure to obtain a solid catalyst powder. The titanium content of the catalyst powder was analyzed by ...

Embodiment 2

[0024] Under nitrogen protection, 2.5 g of MgCl 2 , was added to 100ml of refined methanol and stirred at 60°C for 2 hours to form a uniform transparent solution, and the insoluble impurities were filtered off. to MgCl 2 -Add 10 grams of sodium montmorillonite calcined at 400°C to the methanol solution, continue stirring at 60°C for 2 hours, then filter off excess methanol, and vacuum-dry the reaction system at 60°C for 2 hours. Add 100ml TiCl to the reaction system 4 , stirred at room temperature for 2 hours, filtered off excess TiCl 4 Finally, the solid product was washed 5 times with 50 ml of dry hexane, and dried under reduced pressure to obtain a solid catalyst powder. The titanium content of the catalyst powder was analyzed by ICP to be 1.82wt%.

[0025] Using Al(C 2 h 5 ) 3 As a cocatalyst, [Al] / [Ti]=100 molar ratio, other polymerization conditions and polymer testing conditions are the same as in Example 1. The obtained polymer has a montmorillonite content of ...

Embodiment 3

[0027] Use the catalyst that embodiment 2 prepares, [Al(C 2 h 5 ) 3 ] / [Ti]=3 molar ratio, heptane is solvent, and polymerization temperature is 90 ℃, and other polymerization operating conditions are the same as embodiment 1. The obtained polymer has a montmorillonite content of 4.87wt%, a Vicat heat resistance temperature of 131.1°C and a Young's modulus of 1020MPa.

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Abstract

A montmorillonite-TiCl4 catalyst for preparing the nm-class composition of the olefine polymer or copolymer (polyethylene or polypropylene) contains laminated silicate clay montmorollonite, magnesiumcompound, alcohol compound for dissolving said magnesium compound, TiCl4 and electron providing reagent. Said nm-class composition is prepared by use of saturated paraffin or cycloparaffin as solvent. Its advantages are high teasion strength (32-50 MPa) and low cost.

Description

Technical field: [0001] The invention belongs to the preparation method of montmorillonite-titanium tetrachloride catalyst and polyolefin / montmorillonite composite material. Background technique: [0002] In recent years, organic-inorganic nanocomposites have attracted extensive attention. In particular, nanocomposites of organic polymers and inorganic layered silicate clay minerals have become a research hotspot because of their excellent properties. Polymer clay nanocomposites containing small amounts (<5 wt%) of layered silicate clay exhibit high strength, high modulus, high heat resistance, good barrier properties, and flame retardancy compared to the corresponding pure polymers And better dimensional stability, and basically do not increase the specific gravity of the material. [0003] Polyolefin is the largest and most widely used class of polymers. Polyolefin nanocomposites are of great significance in improving the performance of polyolefins and improving the ...

Claims

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Application Information

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IPC IPC(8): B01J21/06B01J21/16B01J27/135C08F10/00C08F110/02
CPCB01J21/16C08F10/00C08F110/02B01J27/135B01J21/063C08F4/025C08F4/6555C08F4/654
Inventor 张学全杨凤赵海超
Owner CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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