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Method for preparing catalyst of montmorillonite-titanium tetrachloride, and composite material of polyethylene/montmorillonite

A technology of titanium tetrachloride and montmorillonite, which is applied in the field of preparation of polyethylene/montmorillonite composite materials, can solve the problems of low bulk density of polymerization products, difficulty in industrial production, and poor sensitivity of catalyst hydrogenation adjustment, etc., to achieve bulk density High, good mechanical strength and heat resistance, good polymerization activity

Active Publication Date: 2009-12-23
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the hydrogen adjustment sensitivity of the catalyst prepared by this technology is poor, and the bulk density of the polymerization product is low, so it is difficult to put it into industrial production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] 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 to stir at 60° C. for 1 hour, then filter off excess butanol, and wash the solid product three times with 50 ml of dry hexane. Add 100ml dry hexane, 10ml titanium tetrachloride TiCl to the reaction system 4 and 10ml of tetraethyl orthosilicate, stirred at 60°C for 1 hour, and after filtering off the liquid, the solid product was washed 3 times with 50ml of dry hexane. Re-add 100ml TiCl to the reaction system 4 , after stirring at 80 °C for 2 h, the excess TiCl was filtered off 4 , the solid product was washed 5 times with 50 ml of dry hexane, and dried under reduced pressure to obtain a solid catalyst powder. Catalyst powder analysis titan...

Embodiment 2

[0029] Under nitrogen protection, 1.0 g of magnesium dichloride 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 5 grams of sodium montmorillonite calcined at 400°C to the methanol solution, continue to stir at 60°C for 1 hour, then filter off excess butanol, and wash the solid product 3 times with 25ml of dry hexane. Add 50ml dry hexane, 5ml titanium tetrachloride TiCl to the reaction system 4 and 5ml of butyl orthosilicate, stirred at 60°C for 1 hour, and the liquid was filtered off, and the solid product was washed 3 times with 25ml of dry hexane. Re-add 50ml TiCl to the reaction system 4 , after stirring at 80 °C for 2 h, the excess TiCl was filtered off 4 , The solid product was washed 5 times with 25 ml of dry hexane, and dried under reduced pressure to obtain a solid catalyst powder. The titanium content of the catalyst powder was an...

Embodiment 3

[0033] Under nitrogen protection, 5 grams of magnesium dichloride MgCl 2 , was added to 100ml of refined ethanol 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 8 grams of sodium montmorillonite calcined at 400° C. to the ethanol solution, continue to stir at 60° C. for 1 hour, then filter off excess ethanol, and wash the solid product three times with 40 ml of dry hexane. Add 80ml dry hexane, 8ml titanium tetrachloride TiCl to the reaction system 4 and 8ml of tetraethyl orthosilicate, stirred at 60°C for 1 hour, and the liquid was filtered off, and the solid product was washed 3 times with 40ml of dry hexane. Re-add 80ml TiCl to the reaction system 4 , after stirring at 80 °C for 2 h, the excess TiCl was filtered off 4 , The solid product was washed 5 times with 40 ml of dry hexane, and dried under reduced pressure to obtain a solid catalyst powder. The titanium content of the catalys...

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Abstract

A kind of preparation method of montmorillonite-titanium tetrachloride catalyst and polyethylene / montmorillonite composite material thereof, magnesium compound is dissolved in aliphatic alcohol, is mixed with the transparent, stable solution that concentration is 1g-5g / 100ml, presses adding The amount is the ratio of 5-15g montmorillonite / 100ml fatty alcohol, add montmorillonite to magnesium compound fatty alcohol solution, stir at 60°C for 1 hour, filter to remove excess fatty alcohol, then wash with dry hexane for 3 Once, add dry hexane to the reaction system according to the calculated amount of 10ml / g montmorillonite, then add orthosilicate and TiCl4 according to the calculated amount of 1ml / g montmorillonite, stir at 60°C, and at 80°C, according to the calculated Add TiCl4 to the reaction system in an amount of 10ml / g montmorillonite, stir for 2 hours, under the condition of slurry polymerization, use hexane solvent, the [Al] / [Ti] molar ratio is 5-100, and the polymerization temperature is 50-90 ℃. It can be used to prepare nanocomposites of polyethylene and its copolymers, and is suitable for slurry, gas phase and bulk polymerization processes.

Description

Technical field: [0001] The invention relates to a preparation method of a polyethylene / montmorillonite composite material, in particular to a preparation method of a montmorillonite-titanium tetrachloride catalyst and a polyethylene / 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 nanocom...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08L23/06C08K3/34C08F10/02C08F2/44
Inventor 关玉春张学全姜明才蔡洪光
Owner PETROCHINA CO LTD
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